[Objectives]This study was conducted to establish a rapid and effective method for simultaneous extraction of 54 kinds of veterinary drug residues in animal-derived food, including sulfonamides, quinolones, tetracycli...[Objectives]This study was conducted to establish a rapid and effective method for simultaneous extraction of 54 kinds of veterinary drug residues in animal-derived food, including sulfonamides, quinolones, tetracyclines, malachite greens, penicillins, nitroimidazoles, tranquilizers and macrolides, by HPLC-MS. [Methods] The samples were extracted with 80% acetonitrile water(containing 0.1% formic acid), combined with QuEChERS extraction technology and C18 and PSA purification, analyzed by high performance liquid chromatography-mass spectrometry, and quantified by external standard method. The target substances were analyzed on ZORBAX Eclipse C18 chromatographic column using 0.2% formic acid water and 0.2% methanol as mobile phases. The gradient elution mode was used for chromatographic separation and multiple reaction detection. [Results] In the linear range of 0.5-50.0 ng/ml, the linear relationship of the 54 kinds of veterinary drug residues was good, with correlation coefficients(r~2) greater than 0.995, and the detection limits ranged from 0.30 to 1.00 μg/kg. The results showed that the recovery ranged from 75.4% to 118.2% when different matrixes were added for recovery. [Conclusions] This method is simple, efficient, accurate, stable, and highly operable. It is applicable to simultaneous batch screening of veterinary drug residues in animal-derived food, and has high practical application value.展开更多
The degradation of the alkanolamine solvent used in the removal of acid gases from natural gas streams due to exposure to contaminants, thermal degradation and presence of oxygen or oxygen containing compounds will ch...The degradation of the alkanolamine solvent used in the removal of acid gases from natural gas streams due to exposure to contaminants, thermal degradation and presence of oxygen or oxygen containing compounds will change the solvent properties, such as heat transfer coefficient, diffusion coefficient, and mass transfer coefficient of the solvent. Therefore, characterization and quantification of amine degradation product becomes one of the important analyses to determine alkanolamine solvent’s health. In order to identify degradation products of alkanolamine solvent, analytical strategies by using mass spectrometry (MS) as detector have been studied extensively. In this work, due to the low concentration of the amine degradation product, a method was developed for identification of alkanolamine degradation products using LCMS-QTOF technique. A strategy for identification of trace degradation products has been identified. Six (6) alkanolamine degradation products had been identified by using LCMS-QTOF targeted analysis in the blended alkanolamine solvent used in natural gas processing plant. Another fifteen (15) molecular formulas having similarity in chemical structure to alkanolamine degradation products were identified using untargeted analysis strategy, as possible compounds related to degradation products. Using LCMS-QTOF via targeted and untargeted analysis strategy, without tedious column separation and reference standard, enables laboratory to provide a quick and indicative information for alkanolamine solvent’s organic degradation compounds identification in CO<sub>2</sub> adsorption, within reasonable analysis time.展开更多
The major objective of this study was to determine the effect of corn straw or mixed diet on the small molecule metabolites of liver and milk production of healthy Chinese Holstein cows during lactation.In this study,...The major objective of this study was to determine the effect of corn straw or mixed diet on the small molecule metabolites of liver and milk production of healthy Chinese Holstein cows during lactation.In this study,metabolomic methods based on ultra performance liquid chromatography-mass spectrometry(LC-MS)were used to study the liver metabolites of dairy cows fed on corn straw diet or mixed diet.Ten healthy Chinese Holstein cows were randomly assigned to two groups,under the same management condition,fed different diets respectively,corn straw group(CS)or a mixture of alfalfa hay and Chinese wild rye hay mixed forage group(MF).All the cows were fed for 8 weeks and recorded body weight,dry matter intake,body condition score,fat,protein,lactose,milk yield and the total solids.Livers were sampled from each cow through a liver puncture needle for analysis of a significant difference in small molecule metabolites in cow liver samples from the two different diets.The results suggested that different diet types had significant effects on liver metabolism and milk components in dairy cows.The contents of milk fat,the total solids,milk protein,lactose,dry matter intake(DMI),milk yield,milk protein(%),lactose(%)and milk fat(%)of the corn straw group were significantly lower than those of the mixed forage group(p<0.05);the contents of phosphatidylcholine(PC),histidine,hypoxanthine and mridine in liver tissues of the corn straw group were significantly lower than those in the mixed forage group(p<0.05);acetylcarnitine,uric acid,triacylglycerol(TG),acetal phosphatidylcholine(plasmenyl-PC),acetalphosphatidylethanolamine(plasmenyl-PE)and sphingomyelin(SM)of the corn straw group were significantly higher than those in the mixed forage group(p<0.05).In summary,cows fed on mixed forage diet significantly improved milk yield and lactation performance clearly.展开更多
[Objectives] To study the chemical components and relative content of Achyranthes bidentata leaves and provide a scientific basis for further development and utilization of A. bidentata leaves.[Methods] The chemical c...[Objectives] To study the chemical components and relative content of Achyranthes bidentata leaves and provide a scientific basis for further development and utilization of A. bidentata leaves.[Methods] The chemical components of A. bidentata leaves were rapidly analyzed using the ultra high performance liquid chromatography-time of flight-high resolution mass spectrometry (UHPLC-TOF-MS).[Results] Thirty eight chemical compounds were identified in samples of A. bidentata leaves collected from Wen County of Henan Province, in which seven chemical compounds had the relative content higher than 5%, linoleic acid reached 25.7% and inokosterone A reached 13.8%.[Conclusions] A. bidentata leaves contain many kinds of chemical compounds. This study is expected to provide a certain basis for further extraction of linoleic acid and inokosterone A.展开更多
Objective High performance liquid chromatography(HPLC)and liquid chromatography-mass spectrometry(LC/MS)methods were developed for the determination of ganciclovir and its related substances.Methods A Hypersil ODS2 co...Objective High performance liquid chromatography(HPLC)and liquid chromatography-mass spectrometry(LC/MS)methods were developed for the determination of ganciclovir and its related substances.Methods A Hypersil ODS2 column(4.6 mm×250 mm,5 μm)was used with a mobile phase of 0.02 M potassium dihydrogen phosphate buffer(pH 6.0)-methanol(92∶8)at a flow rate of 1.0 mL/min,and UV detector set at 254 nm was used for monitoring the eluents.Results The method was simple,rapid,selective and capable of separating all related substances at trace level with a detection limit of 0.04 μg/mL.It has been validated with respect to accuracy,precision,linearity,and limits of detection and quantification.The linearity range was 10.2-153.0 μg/mL with r=0.9998.The percentage recoveries ranged from 96.7% to 101.6%,and RSD was 1.24%-1.96%(n=5).Conclusion The method was found to be suitable not only for monitoring the reactions during the process development but also for quality control of ganciclovir.For identification of related substances,LC/MS was used.The mainly related substances of ganciclovir active pharmaceutical ingredients(API)were determined as guanine,(1,3-dioxolan-4-yl)methyl acetate,and diacetyl guanine.展开更多
A simple, accurate and sensitive method for characterization of pentachlorophenol in soil was presented. The method included Soxhlet extraction using extracting agent of methanol/water/triethylamine (80∶20∶2), decon...A simple, accurate and sensitive method for characterization of pentachlorophenol in soil was presented. The method included Soxhlet extraction using extracting agent of methanol/water/triethylamine (80∶20∶2), decontamination using solid-phase extraction (SPE) column and characterization by liquid chromatography-mass spectrometry (LCMS). The developed analytical method was successfully used to the determination of pentachlorophenol in soil samples.展开更多
In the present study, we developed and validated an analytical method using ultra performance liquid chromatography-mass spectrometry (UPLC/MS) for the quantitative determination of 2,2',4,4'-tetrabromodipheny...In the present study, we developed and validated an analytical method using ultra performance liquid chromatography-mass spectrometry (UPLC/MS) for the quantitative determination of 2,2',4,4'-tetrabromodiphenyl ether (BDE-47) metabolism by rat hepatic microsomes. BDE-47 is a brominated flame retardant that was widely used in a variety of consumer products and has subsequently been identified as a ubiquitous environmental contaminant. Hydroxy-bromodiphenyl ethers (OH-BDEs) were isolated from rat hepatic microsomes by liquid-liquid extraction. Chromatographic separation was achieved by UPLC on a C18 column with gradient elution using a mobile phase consisting of methanol and water, each containing 0.1% formic acid, at a flow rate of 0.2 mL/min. Detection and quantification were performed using a mass spectrometer in single ion recording mode with negative electrospray ionization. The UPLC/MS method was validated for linearity, limit of quantification (LOQ), accuracy, precision and recovery. The weighted calibration curves (1/X2) were linear over a concentration range of 5 - 250 nM with LOQ values between 5 nM and 50 nM for the individual OH-BDEs. Intra- and inter- day accuracy (%DEV) and precision (%RSD) values ranged from –11.7% to 9.5% and 5.9% to 16.5%, respectively. Recovery values of 70% to 90% were obtained for all OH-BDEs. The validated method allowed us to successfully analyze metabolite formation following incubation of BDE-47 with hepatic microsomes prepared from phenobarbital-treated rats. Results demonstrate that the UPLC/MS method has sufficient sensitivity and reproducibility to fully characterize the in vitro metabolism of BDE-47 and possibly other PBDEs.展开更多
Objective: To investigate the changes in the hypothalamic metabolites of lipopolysaccharide(LPS) febrile young rabbits after the treatment with pediatric tuina.Methods: A total of 30 young rabbits were randomly assign...Objective: To investigate the changes in the hypothalamic metabolites of lipopolysaccharide(LPS) febrile young rabbits after the treatment with pediatric tuina.Methods: A total of 30 young rabbits were randomly assigned into three groups: the normal group, the model group, and the tuina group. Both the model group and the tuina group were injected intravenously with LPS. “Six antipyretic manipulations”(pushing Tianmen, pushing Kangong, kneading Taiyang,kneading Erhougaogu, clearing Tianheshui, and pushing Jizhu) were administered 1 h after the LPS injection in the tuina group. The rectal temperatures of the young rabbits were monitored during the experiment to explore the antipyretic effect. Three hours after the injection, the content of interleukin-1β(IL-1β), tumor necrosis factor(TNF)-a, and prostaglandin E;(PGE;) in the serum was detected. In addition, liquid chromatography-mass spectrometry(LC-MS) was used for the hypothalamus metabolomics.Results: Compared with the model group, the rectal temperature of the tuina group was decreased at 2 h and 3 h after the LPS injection(P =.04, P =.03, respectively), and the content of IL-1β, TNF-a, and PGE2was decreased(P =.03, P =.003, and P =.008, respectively). The metabolomics results showed that there were 23 potential biomarkers after the tuina intervention, enriching 27 pathways. Lipid metabolites,especially glycerophospholipids, were a majority of the altered metabolites. The primary metabolic pathways affected by tuina included the arachidonic acid metabolism, the GABAergic synapse, D-glutamine and D-glutamate metabolism, and the glutamatergic synapse.Conclusion: Pediatric tuina reduced the temperature of the febrile rabbits and downregulated the expression of IL-1β, TNF-a, and PGE2, and the antipyretic mechanism may be related to changes in metabolites and metabolic pathways in the hypothalamus.展开更多
Objectives of the research to present a modern theory of water purification for multiple purposes entitled “a novelties filtration theory of liquid chromatography-mass spectrometry” is an exceedingly sensitive and s...Objectives of the research to present a modern theory of water purification for multiple purposes entitled “a novelties filtration theory of liquid chromatography-mass spectrometry” is an exceedingly sensitive and specific analytical technique in volume layers woven fabrics that can precisely determine the identities and quantities of compounds within volume Nanotube of cotton filament of layers woven fabrics. The problems are that the filters in the local and international markets have increased complications in configuration, installation and cost without reaching the efficiency that humanity hopes. Throw materials and methods the chromatography-mass spectrometry in layers woven fabrics, and throw the nanotube of cotton filament for purification of water dyes and smells. Industry, in which mass spectrometry is a convenient, versatile method for characterization and identification of process throw the Nanotube of cotton filament for purification of water dyes and smells. Results came up with a theme “innovations in textiles”, and also, for characterization of fibers and contaminants of the fabrics. Additive manufacturing in layers woven fabrics, are the processes used to synthesize a volume object under computer control with successive material layers that have been used and highlighted. The conclusions has included chromatography-mass spectrometry drop, physico-chemical, biological, combined physical-biological and chemical-biological treatment processes recently being developed to meet Jet-filtration, the strict discharging limits set by ASTM standards. Some important aspects of both qualitative and quantitative data analysis have been described and the power of using mass profiles to enhance selectivity and sensitivity has been demonstrated.展开更多
To identify the species in liquid surface using mass spectrometry,we must eliminate or reduce interferences during the vaporization or desorption of the species from the liquid surface.It is much more challenging to i...To identify the species in liquid surface using mass spectrometry,we must eliminate or reduce interferences during the vaporization or desorption of the species from the liquid surface.It is much more challenging to isolate the ionic,larger species from the liquid surface,because of the frangible structures and the higher solvation energies of those species.Here we demonstrate a new mass spectrometry in which the ionic species at the liquid surface can be desorbed with ultrasoft infrared picosecond laser pulses while the liquid surface is not breached.This laser desorption assisted mass spectrometry is not only a powerful tool to detect the fragile species but also promising to investigate vibrational energy transfer dynamics in the liquid surface.展开更多
[Objectives]This study was conducted to purify mutton samples by gel permeation chromatography(GPC).[Methods]Fourteen organophosphorus pesticide residues in samples were qualitatively and quantitatively analyzed by ga...[Objectives]This study was conducted to purify mutton samples by gel permeation chromatography(GPC).[Methods]Fourteen organophosphorus pesticide residues in samples were qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry(GC-MS)in selective ion scanning mode(SIM).[Results]The organophosphorus pesticide standard solutions showed good linearity in the mass concentration range of 0.1-10.0μg/ml with correlation coefficients(r)not lower than 0.999,and the detection limits(S=3 N)ranged from 0.01 to 0.05 mg/kg.The average recovery values were in the range of 80.2%-99.7%,with relative standard deviations(RSDs,n=3)in the range of 1.8%-6.3%,at the addition levels of 0.5,1.0 and 2.0 mg/kg.[Conclusions]The method is simple,sensitive and accurate,and can be used for the determination of organophosphorus pesticide residues in mutton.展开更多
Traditional Chinese medicine(TCM) has been an indispensable source of drugs for curing various human diseases.However,the inherent chemical diversity and complexity of TCM restricted the safety and efficacy of its usa...Traditional Chinese medicine(TCM) has been an indispensable source of drugs for curing various human diseases.However,the inherent chemical diversity and complexity of TCM restricted the safety and efficacy of its usage.Over the past few decades,the combination of liquid chromatography with mass spectrometry has contributed greatly to the TCM qualitative analysis.And novel approaches have been continuously introduced to improve the analytical performance,including both the data acquisition methods to generate a large and informative dataset,and the data post-processing tools to extract the structure-related MS information.Furthermore,the fast-developing computer techniques and big data analytics have markedly enriched the data processing tools,bringing benefits of high efficiency and accuracy.To provide an up-to-date review of the latest techniques on the TCM qualitative analysis,multiple data-independent acquisition methods and data-dependent acquisition methods(precursor ion list,dynamic exclusion,mass tag,precursor ion scan,neutral loss scan,and multiple reaction monitoring)and post-processing techniques(mass defect filtering,diagnostic ion filtering,neutral loss filtering,mass spectral trees similarity filter,molecular networking,statistical analysis,database matching,etc.) were summarized and categorized.Applications of each technique and integrated analytical strategies were highlighted,discussion and future perspectives were proposed as well.展开更多
Metabolite analysis or metabolomics is an important component of systems biology in the post-genomic era.Although separate liquid chromatography(LC) methods for quantification of the major classes of polar metabolit...Metabolite analysis or metabolomics is an important component of systems biology in the post-genomic era.Although separate liquid chromatography(LC) methods for quantification of the major classes of polar metabolites of plants have been available for decades,a single method that enables simultaneous determination of hundreds of polar metabolites is possible only with gas chromatography-mass spectrometry(GC-MS) techniques.The rapid expansion of new LC stationary phases in the market and the ready access of mass spectrometry in many laboratories provides an excellent opportunity for developing LC-MS based methods for multitarget quantification of polar metabolites.Although various LC-MS methods have been developed over the last 10 years with the aim to quantify one or more classes of polar compounds in different matrices,currently there is no consensus LC-MS method that is widely used in plant metabolomics studies.The most promising methods applicable to plant metabolite analysis will be reviewed in this paper and the major problems encountered highlighted.The aim of this review is to provide plant scientists,with limited to moderate experience in analytical chemistry,with up-to-date and simplified information regarding the current status of polar metabolite analysis using LC-MS techniques.展开更多
Objective:To study the differences between the serum metabolites in patients with adenomatous polyps of the colon and yang-deficiency constitution and those without colon polyps and with balanced constitution,and look...Objective:To study the differences between the serum metabolites in patients with adenomatous polyps of the colon and yang-deficiency constitution and those without colon polyps and with balanced constitution,and look for biomarkers that can be used to distinguish between the two groups.Methods:General patient information was gathered,and Chinese medicine constitutions were collected in 940 patients who underwent electronic colonoscopy.A total of 119 patients with adenomatous polyps of the colon and yang-deficiency constitution were included in the experimental group,and 150 patients without colon polyps and with balanced constitution were included in the control group.Metabolomics analysis was performed on the fasting venous blood obtained from each patient in both groups.Principal component analysis and orthogonal partial least squares discriminant analysis were performed on the detection results,potential biomarkers were screened,metabolic pathway changes were determined,and the metabolic processes involved were discussed.Results:A total of 59 differential biomarkers between the experimental group and the control group were identified.The differential metabolites were found mainly in the glycerophospholipid metabolism pathway,and the bile acid 3-oxo-4,6-choladienoic acid was the biomarker that distinguished the experimental group from the control group.Conclusions:With the help of metabolomics analysis,the differential metabolites in patients with adenomatous polyps of the colon and yang-deficiency constitution and those in patients without colon polyps and with balanced constitution could be identified.The biomarker 3-oxo-4,6-choladienoic acid may have potential diagnostic value in patients with adenomatous polyp of the colon and yang-deficiency constitution.(Trial Registration No.NCT02986308)展开更多
Objective:The objective of the study was to develop a rapid and sensitive ultra-performance liquid chromatography-tandem mass spectrometric method for the determination of tetrandrine,fangchinoline,and cyclanoline in ...Objective:The objective of the study was to develop a rapid and sensitive ultra-performance liquid chromatography-tandem mass spectrometric method for the determination of tetrandrine,fangchinoline,and cyclanoline in rat plasma and to investigate their pharmacokinetics after oral administration of Stephaniae Tetrandrae Radix extracts.Methods:Sample pretreatment involved methanol pretreatment and liquid–liquid extraction of ethyl acetate from plasma with methanol.Tramadol was used as the internal standard.The analysis was performed using an high strength silica T3 column(100 mm×2.1 mm,1.8μm)and a gradient elution method consisting of mobile phase solution A(0.1%formic acid in water)and B(acetonitrile)at a flow rate of 0.4 mL/min.The detection was performed using a triple quadrupole tandem mass spectrometer in the multiple reaction monitoring mode and using an electrospray ionization source in the positive ionization mode.Results:High efficiency was achieved with an analysis time of 4 min/sample.The calibration curve linear in the concentration range of 1250 ng/ml(R^(2)≥0.9900)and the lower limit of quantification is 1 ng/ml.The intraday and interday precision(relative standard deviation)values were lower than 9.4.Accuracy(relative error)was within 10.3%at all three quality control levels.Conclusions:This method was successfully applied in pharmacokinetics of tetrandrine,fangchinoline,and cyclanoline in rats after oral administration of Stephaniae Tetrandrae Radix extracts.The maximum plasma concentration(C_(max))of tetrandrine,fangchinoline,and cyclanoline was 124.71±16.08,84.56±3.28,and 57.61±6.26 ng/mL,respectively.The time to reach C_(max)was 10.39±3.04 for tetrandrine,10.17±3.04 for fangchinoline,and 6.40±3.16 for cyclanoline.The pharmacokinetic results might help further guide the clinical application of Stephaniae Tetrandrae Radix.展开更多
A new liquid chromatography-mass spectrometry method for the determination of carbamazepine,clonazepam,alprazolam,estazolam and phenytoin in human plasma has been developed by using diazepam as an internal standard.Ch...A new liquid chromatography-mass spectrometry method for the determination of carbamazepine,clonazepam,alprazolam,estazolam and phenytoin in human plasma has been developed by using diazepam as an internal standard.Chromatographic separation was performed on a Zorbax SB-C18 column(30 mm × 2.1 mm,3.5 ?m) with a mobile phase consisting of methanol and aqueous 25 mM ammonium acetate using gradient elution.A diethyl ether extraction method was used for the extraction of five anti-epilepsy drugs.The final extract was injected for analysis by LC-MS/MS.The method was validated within the concentration range of 50-5000 ng mL-1 for five anti-epilepsy drugs.The precision of the assay(RSD%) was less than 10% at all concentration levels within the tested range.The method recoveries for all samples were more than 90%.The results indicate that the method is specific,sensitive and accurate,and suitable to study the pharmacokinetics,to adjust the dosage for individual administration,and to monitor the drug-concentration and drug abuse of the five anti-epilepsy drugs.展开更多
A sensitive, accurate and robust Liquid Chromatography Tandem Mass Spectrometry method has been developed and validated to measure voriconazole trough levels in human plasma. The plasma samples were mixed with flucona...A sensitive, accurate and robust Liquid Chromatography Tandem Mass Spectrometry method has been developed and validated to measure voriconazole trough levels in human plasma. The plasma samples were mixed with fluconazole as an Internal Standard and directed to protein precipitation and drug extraction. An aliquot of 1 μl was injected into the chromatographic system and separated by the Acquity BEH C18 column at a flow rate of 0.30 ml/min in a gradient mobile phase consisting of acetonitrile, Ultrapure water (UPW), methanol and formic acid. Voriconazole was detected by a Triple Quadrupole Detector (TQD) operating on Multiple Reaction Monitoring (MRM) and a positive ion mode Electrospray ionization (ESI) Q1 mass: 350.1 m/z, Q3 mass: 281.1 m/z. Method linearity of the calibration curve (0.10 - 8.00 μg/ml) indicated a correlation coefficient r ≥ 0.99. The intra and inter-assay accuracy was within 85% - 115% and the intra and inter-assay precision was ≤5.76%. Voriconazole recovery percentage was between 97.69 - 119.62%. The method was successively applied in routine voriconazole TDM.展开更多
The aim of this work was to develop a liquid chromatography-tandem mass spectrometry method for the determination of milk allergen and egg allergen in food products.Signature peptides GGLEPINFQTAADQAR,VGINYWLAHK,VLVLD...The aim of this work was to develop a liquid chromatography-tandem mass spectrometry method for the determination of milk allergen and egg allergen in food products.Signature peptides GGLEPINFQTAADQAR,VGINYWLAHK,VLVLDTDYK,FFVAPFPEVFGK,and NAVPITPTLNR were confirmed and synthesized as the quantitative peptide of ovalbumin,α-lactalbumin,β-lactoglobulin,α_(S1)-casein andα_(S2)-casein,the relative isotope-labeled internal standards were used in the quantitative analysis.Linear range was in the range of0.5-5000.0 nmol/L for egg and milk allergen in bread,cake,cookie,rice crust and wheat flour samples with free from egg and milk,the limits of detection of milk allergens and egg allergen were in the range between0.94 mg/100 g and 56.71 mg/100 g,limits of quantification of milk allergens and egg allergen were in the range between 2.36 mg/100 g and 141.78 mg/100 g.The recoveries ranged from 76.7%to 122.8%,the relative standard deviations were in the range of 1.60%-15.60%.The developed method has been successfully used for the detection of egg and milk allergen in various food samples.展开更多
A simple and rapid technique based on liquid-liquid extraction coupled to gas chromatography-mass spectrometric detection(LLE-GC-MS) was developed for analysis of taste and odour compound β-ionone in water. Instrumen...A simple and rapid technique based on liquid-liquid extraction coupled to gas chromatography-mass spectrometric detection(LLE-GC-MS) was developed for analysis of taste and odour compound β-ionone in water. Instrument parameters including programmed oven temperature, injection temperature and ion source temperature were evaluated and optimized. Effects of extraction time, ionic strength and p H on the detection efficiency were investigated and optimum conditions were 8 min of extraction time, without Na Cl addition at p H=9. Good linearity(R2=0.9997) was obtained when the linear range was 10-500 μg/L. The recoveries of β-ionone in ultrapure water and tap water samples were 88%-95% and 110%-114%, respectively. The relative standard deviations(RSD) were less than 10%. The method detection limit(MDL) and rejection quality level(RQL) were achieved at1.98 μg/L and 6.53 μg/L, respectively. LLE-GC-MS was demonstrated to be a rapid and convenient method for the determination ofβ-ionone in water samples.展开更多
[Objectives]A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was established for the determination of 14β-receptor agonist residues in mutton.[Methods]Samples were hydrolyzed byβ-g...[Objectives]A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was established for the determination of 14β-receptor agonist residues in mutton.[Methods]Samples were hydrolyzed byβ-glucuronidase and extracted with 5%acetic acid-acetonitrile(1:99,V/V)solution.An Eclipse plus C 18 column was used for separation,and the MRM mode was used for qualitative analysis,and the external standard method was used for quantitative analysis of matrix standard solutions.[Results]Under the optimal conditions,the retention time of the 14 kinds ofβ-receptor agonists ranged from 1.0 to 9.5 min.When the mass concentration was in the range of 0.05-0.50μg/ml,the linear relationship ofβ-receptor agonists was good,with correlation coefficients(r)≥0.9992.The detection limits of the method were in the range of 0.04-0.87μg/kg,and the quantitative limits were in the range of 0.35-1.86μg/kg.The average recovery values were in the range of 82.8%-108.9%,with RSDs(n=6)in the range of 1.9%-6.7%.[Conclusions]The method is simple,sensitive,reproducible,accurate,and can be used for simultaneous determination of the 14 kinds ofβ-receptor agonist residues in mutton.展开更多
文摘[Objectives]This study was conducted to establish a rapid and effective method for simultaneous extraction of 54 kinds of veterinary drug residues in animal-derived food, including sulfonamides, quinolones, tetracyclines, malachite greens, penicillins, nitroimidazoles, tranquilizers and macrolides, by HPLC-MS. [Methods] The samples were extracted with 80% acetonitrile water(containing 0.1% formic acid), combined with QuEChERS extraction technology and C18 and PSA purification, analyzed by high performance liquid chromatography-mass spectrometry, and quantified by external standard method. The target substances were analyzed on ZORBAX Eclipse C18 chromatographic column using 0.2% formic acid water and 0.2% methanol as mobile phases. The gradient elution mode was used for chromatographic separation and multiple reaction detection. [Results] In the linear range of 0.5-50.0 ng/ml, the linear relationship of the 54 kinds of veterinary drug residues was good, with correlation coefficients(r~2) greater than 0.995, and the detection limits ranged from 0.30 to 1.00 μg/kg. The results showed that the recovery ranged from 75.4% to 118.2% when different matrixes were added for recovery. [Conclusions] This method is simple, efficient, accurate, stable, and highly operable. It is applicable to simultaneous batch screening of veterinary drug residues in animal-derived food, and has high practical application value.
文摘The degradation of the alkanolamine solvent used in the removal of acid gases from natural gas streams due to exposure to contaminants, thermal degradation and presence of oxygen or oxygen containing compounds will change the solvent properties, such as heat transfer coefficient, diffusion coefficient, and mass transfer coefficient of the solvent. Therefore, characterization and quantification of amine degradation product becomes one of the important analyses to determine alkanolamine solvent’s health. In order to identify degradation products of alkanolamine solvent, analytical strategies by using mass spectrometry (MS) as detector have been studied extensively. In this work, due to the low concentration of the amine degradation product, a method was developed for identification of alkanolamine degradation products using LCMS-QTOF technique. A strategy for identification of trace degradation products has been identified. Six (6) alkanolamine degradation products had been identified by using LCMS-QTOF targeted analysis in the blended alkanolamine solvent used in natural gas processing plant. Another fifteen (15) molecular formulas having similarity in chemical structure to alkanolamine degradation products were identified using untargeted analysis strategy, as possible compounds related to degradation products. Using LCMS-QTOF via targeted and untargeted analysis strategy, without tedious column separation and reference standard, enables laboratory to provide a quick and indicative information for alkanolamine solvent’s organic degradation compounds identification in CO<sub>2</sub> adsorption, within reasonable analysis time.
基金Supported by the National Natural Science Foundation of China(31101784)Funds for Young Researchers from Northeast Agricultural University(14QC43)。
文摘The major objective of this study was to determine the effect of corn straw or mixed diet on the small molecule metabolites of liver and milk production of healthy Chinese Holstein cows during lactation.In this study,metabolomic methods based on ultra performance liquid chromatography-mass spectrometry(LC-MS)were used to study the liver metabolites of dairy cows fed on corn straw diet or mixed diet.Ten healthy Chinese Holstein cows were randomly assigned to two groups,under the same management condition,fed different diets respectively,corn straw group(CS)or a mixture of alfalfa hay and Chinese wild rye hay mixed forage group(MF).All the cows were fed for 8 weeks and recorded body weight,dry matter intake,body condition score,fat,protein,lactose,milk yield and the total solids.Livers were sampled from each cow through a liver puncture needle for analysis of a significant difference in small molecule metabolites in cow liver samples from the two different diets.The results suggested that different diet types had significant effects on liver metabolism and milk components in dairy cows.The contents of milk fat,the total solids,milk protein,lactose,dry matter intake(DMI),milk yield,milk protein(%),lactose(%)and milk fat(%)of the corn straw group were significantly lower than those of the mixed forage group(p<0.05);the contents of phosphatidylcholine(PC),histidine,hypoxanthine and mridine in liver tissues of the corn straw group were significantly lower than those in the mixed forage group(p<0.05);acetylcarnitine,uric acid,triacylglycerol(TG),acetal phosphatidylcholine(plasmenyl-PC),acetalphosphatidylethanolamine(plasmenyl-PE)and sphingomyelin(SM)of the corn straw group were significantly higher than those in the mixed forage group(p<0.05).In summary,cows fed on mixed forage diet significantly improved milk yield and lactation performance clearly.
基金Supported by Key Scientific and Technological Research Project in Higher Education Institutions of Henan Province(17A350002)Project of National Natural Science Foundation of China(81172953)
文摘[Objectives] To study the chemical components and relative content of Achyranthes bidentata leaves and provide a scientific basis for further development and utilization of A. bidentata leaves.[Methods] The chemical components of A. bidentata leaves were rapidly analyzed using the ultra high performance liquid chromatography-time of flight-high resolution mass spectrometry (UHPLC-TOF-MS).[Results] Thirty eight chemical compounds were identified in samples of A. bidentata leaves collected from Wen County of Henan Province, in which seven chemical compounds had the relative content higher than 5%, linoleic acid reached 25.7% and inokosterone A reached 13.8%.[Conclusions] A. bidentata leaves contain many kinds of chemical compounds. This study is expected to provide a certain basis for further extraction of linoleic acid and inokosterone A.
文摘Objective High performance liquid chromatography(HPLC)and liquid chromatography-mass spectrometry(LC/MS)methods were developed for the determination of ganciclovir and its related substances.Methods A Hypersil ODS2 column(4.6 mm×250 mm,5 μm)was used with a mobile phase of 0.02 M potassium dihydrogen phosphate buffer(pH 6.0)-methanol(92∶8)at a flow rate of 1.0 mL/min,and UV detector set at 254 nm was used for monitoring the eluents.Results The method was simple,rapid,selective and capable of separating all related substances at trace level with a detection limit of 0.04 μg/mL.It has been validated with respect to accuracy,precision,linearity,and limits of detection and quantification.The linearity range was 10.2-153.0 μg/mL with r=0.9998.The percentage recoveries ranged from 96.7% to 101.6%,and RSD was 1.24%-1.96%(n=5).Conclusion The method was found to be suitable not only for monitoring the reactions during the process development but also for quality control of ganciclovir.For identification of related substances,LC/MS was used.The mainly related substances of ganciclovir active pharmaceutical ingredients(API)were determined as guanine,(1,3-dioxolan-4-yl)methyl acetate,and diacetyl guanine.
基金This work was supported by the fund of the Science and Technology Commission of Ningbo (NB 2002009)
文摘A simple, accurate and sensitive method for characterization of pentachlorophenol in soil was presented. The method included Soxhlet extraction using extracting agent of methanol/water/triethylamine (80∶20∶2), decontamination using solid-phase extraction (SPE) column and characterization by liquid chromatography-mass spectrometry (LCMS). The developed analytical method was successfully used to the determination of pentachlorophenol in soil samples.
文摘In the present study, we developed and validated an analytical method using ultra performance liquid chromatography-mass spectrometry (UPLC/MS) for the quantitative determination of 2,2',4,4'-tetrabromodiphenyl ether (BDE-47) metabolism by rat hepatic microsomes. BDE-47 is a brominated flame retardant that was widely used in a variety of consumer products and has subsequently been identified as a ubiquitous environmental contaminant. Hydroxy-bromodiphenyl ethers (OH-BDEs) were isolated from rat hepatic microsomes by liquid-liquid extraction. Chromatographic separation was achieved by UPLC on a C18 column with gradient elution using a mobile phase consisting of methanol and water, each containing 0.1% formic acid, at a flow rate of 0.2 mL/min. Detection and quantification were performed using a mass spectrometer in single ion recording mode with negative electrospray ionization. The UPLC/MS method was validated for linearity, limit of quantification (LOQ), accuracy, precision and recovery. The weighted calibration curves (1/X2) were linear over a concentration range of 5 - 250 nM with LOQ values between 5 nM and 50 nM for the individual OH-BDEs. Intra- and inter- day accuracy (%DEV) and precision (%RSD) values ranged from –11.7% to 9.5% and 5.9% to 16.5%, respectively. Recovery values of 70% to 90% were obtained for all OH-BDEs. The validated method allowed us to successfully analyze metabolite formation following incubation of BDE-47 with hepatic microsomes prepared from phenobarbital-treated rats. Results demonstrate that the UPLC/MS method has sufficient sensitivity and reproducibility to fully characterize the in vitro metabolism of BDE-47 and possibly other PBDEs.
基金supported by the National Natural Science Foundation of China (81873392)the Beijing Natural Science Foundation (7192113)
文摘Objective: To investigate the changes in the hypothalamic metabolites of lipopolysaccharide(LPS) febrile young rabbits after the treatment with pediatric tuina.Methods: A total of 30 young rabbits were randomly assigned into three groups: the normal group, the model group, and the tuina group. Both the model group and the tuina group were injected intravenously with LPS. “Six antipyretic manipulations”(pushing Tianmen, pushing Kangong, kneading Taiyang,kneading Erhougaogu, clearing Tianheshui, and pushing Jizhu) were administered 1 h after the LPS injection in the tuina group. The rectal temperatures of the young rabbits were monitored during the experiment to explore the antipyretic effect. Three hours after the injection, the content of interleukin-1β(IL-1β), tumor necrosis factor(TNF)-a, and prostaglandin E;(PGE;) in the serum was detected. In addition, liquid chromatography-mass spectrometry(LC-MS) was used for the hypothalamus metabolomics.Results: Compared with the model group, the rectal temperature of the tuina group was decreased at 2 h and 3 h after the LPS injection(P =.04, P =.03, respectively), and the content of IL-1β, TNF-a, and PGE2was decreased(P =.03, P =.003, and P =.008, respectively). The metabolomics results showed that there were 23 potential biomarkers after the tuina intervention, enriching 27 pathways. Lipid metabolites,especially glycerophospholipids, were a majority of the altered metabolites. The primary metabolic pathways affected by tuina included the arachidonic acid metabolism, the GABAergic synapse, D-glutamine and D-glutamate metabolism, and the glutamatergic synapse.Conclusion: Pediatric tuina reduced the temperature of the febrile rabbits and downregulated the expression of IL-1β, TNF-a, and PGE2, and the antipyretic mechanism may be related to changes in metabolites and metabolic pathways in the hypothalamus.
文摘Objectives of the research to present a modern theory of water purification for multiple purposes entitled “a novelties filtration theory of liquid chromatography-mass spectrometry” is an exceedingly sensitive and specific analytical technique in volume layers woven fabrics that can precisely determine the identities and quantities of compounds within volume Nanotube of cotton filament of layers woven fabrics. The problems are that the filters in the local and international markets have increased complications in configuration, installation and cost without reaching the efficiency that humanity hopes. Throw materials and methods the chromatography-mass spectrometry in layers woven fabrics, and throw the nanotube of cotton filament for purification of water dyes and smells. Industry, in which mass spectrometry is a convenient, versatile method for characterization and identification of process throw the Nanotube of cotton filament for purification of water dyes and smells. Results came up with a theme “innovations in textiles”, and also, for characterization of fibers and contaminants of the fabrics. Additive manufacturing in layers woven fabrics, are the processes used to synthesize a volume object under computer control with successive material layers that have been used and highlighted. The conclusions has included chromatography-mass spectrometry drop, physico-chemical, biological, combined physical-biological and chemical-biological treatment processes recently being developed to meet Jet-filtration, the strict discharging limits set by ASTM standards. Some important aspects of both qualitative and quantitative data analysis have been described and the power of using mass profiles to enhance selectivity and sensitivity has been demonstrated.
基金supported by the Strategic Priority Research Program of the Chinese Academy of Sciences(No.XDB0450202).
文摘To identify the species in liquid surface using mass spectrometry,we must eliminate or reduce interferences during the vaporization or desorption of the species from the liquid surface.It is much more challenging to isolate the ionic,larger species from the liquid surface,because of the frangible structures and the higher solvation energies of those species.Here we demonstrate a new mass spectrometry in which the ionic species at the liquid surface can be desorbed with ultrasoft infrared picosecond laser pulses while the liquid surface is not breached.This laser desorption assisted mass spectrometry is not only a powerful tool to detect the fragile species but also promising to investigate vibrational energy transfer dynamics in the liquid surface.
基金Supported by The Fourth Batch of High-end Talent Project in Hebei Province.
文摘[Objectives]This study was conducted to purify mutton samples by gel permeation chromatography(GPC).[Methods]Fourteen organophosphorus pesticide residues in samples were qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry(GC-MS)in selective ion scanning mode(SIM).[Results]The organophosphorus pesticide standard solutions showed good linearity in the mass concentration range of 0.1-10.0μg/ml with correlation coefficients(r)not lower than 0.999,and the detection limits(S=3 N)ranged from 0.01 to 0.05 mg/kg.The average recovery values were in the range of 80.2%-99.7%,with relative standard deviations(RSDs,n=3)in the range of 1.8%-6.3%,at the addition levels of 0.5,1.0 and 2.0 mg/kg.[Conclusions]The method is simple,sensitive and accurate,and can be used for the determination of organophosphorus pesticide residues in mutton.
基金financially supported by National Key R&D Program of China (2018YFC1707900, 2019YFC1711000, and 2019YFC1711400)National Natural Science Foundation of China (82003938)+1 种基金State Key Program of National Natural Science Foundation of China (81530095)Qi-Huang Scholar of National Traditional Chinese Medicine Leading Talents Support Program (2018)。
文摘Traditional Chinese medicine(TCM) has been an indispensable source of drugs for curing various human diseases.However,the inherent chemical diversity and complexity of TCM restricted the safety and efficacy of its usage.Over the past few decades,the combination of liquid chromatography with mass spectrometry has contributed greatly to the TCM qualitative analysis.And novel approaches have been continuously introduced to improve the analytical performance,including both the data acquisition methods to generate a large and informative dataset,and the data post-processing tools to extract the structure-related MS information.Furthermore,the fast-developing computer techniques and big data analytics have markedly enriched the data processing tools,bringing benefits of high efficiency and accuracy.To provide an up-to-date review of the latest techniques on the TCM qualitative analysis,multiple data-independent acquisition methods and data-dependent acquisition methods(precursor ion list,dynamic exclusion,mass tag,precursor ion scan,neutral loss scan,and multiple reaction monitoring)and post-processing techniques(mass defect filtering,diagnostic ion filtering,neutral loss filtering,mass spectral trees similarity filter,molecular networking,statistical analysis,database matching,etc.) were summarized and categorized.Applications of each technique and integrated analytical strategies were highlighted,discussion and future perspectives were proposed as well.
基金funded by the Dairy Futures Co-operative Research Centre
文摘Metabolite analysis or metabolomics is an important component of systems biology in the post-genomic era.Although separate liquid chromatography(LC) methods for quantification of the major classes of polar metabolites of plants have been available for decades,a single method that enables simultaneous determination of hundreds of polar metabolites is possible only with gas chromatography-mass spectrometry(GC-MS) techniques.The rapid expansion of new LC stationary phases in the market and the ready access of mass spectrometry in many laboratories provides an excellent opportunity for developing LC-MS based methods for multitarget quantification of polar metabolites.Although various LC-MS methods have been developed over the last 10 years with the aim to quantify one or more classes of polar compounds in different matrices,currently there is no consensus LC-MS method that is widely used in plant metabolomics studies.The most promising methods applicable to plant metabolite analysis will be reviewed in this paper and the major problems encountered highlighted.The aim of this review is to provide plant scientists,with limited to moderate experience in analytical chemistry,with up-to-date and simplified information regarding the current status of polar metabolite analysis using LC-MS techniques.
文摘Objective:To study the differences between the serum metabolites in patients with adenomatous polyps of the colon and yang-deficiency constitution and those without colon polyps and with balanced constitution,and look for biomarkers that can be used to distinguish between the two groups.Methods:General patient information was gathered,and Chinese medicine constitutions were collected in 940 patients who underwent electronic colonoscopy.A total of 119 patients with adenomatous polyps of the colon and yang-deficiency constitution were included in the experimental group,and 150 patients without colon polyps and with balanced constitution were included in the control group.Metabolomics analysis was performed on the fasting venous blood obtained from each patient in both groups.Principal component analysis and orthogonal partial least squares discriminant analysis were performed on the detection results,potential biomarkers were screened,metabolic pathway changes were determined,and the metabolic processes involved were discussed.Results:A total of 59 differential biomarkers between the experimental group and the control group were identified.The differential metabolites were found mainly in the glycerophospholipid metabolism pathway,and the bile acid 3-oxo-4,6-choladienoic acid was the biomarker that distinguished the experimental group from the control group.Conclusions:With the help of metabolomics analysis,the differential metabolites in patients with adenomatous polyps of the colon and yang-deficiency constitution and those in patients without colon polyps and with balanced constitution could be identified.The biomarker 3-oxo-4,6-choladienoic acid may have potential diagnostic value in patients with adenomatous polyp of the colon and yang-deficiency constitution.(Trial Registration No.NCT02986308)
基金financially supported by National Natural Science Foundation of China/81973439Heilongjiang University of Chinese Medicine Research Fund/201504+4 种基金National Natural Science Foundation of China/81803686Research Fund of Heilongjiang University of Traditional Chinese Medicine/201504Heilongjiang Postdoctoral Research Start-up Funding Project/LBH-Q16214Heilongjiang Science Foundation Project/H2018056Heilongjiang University of Traditional Medicine Talents Support Plan/2018RCD03。
文摘Objective:The objective of the study was to develop a rapid and sensitive ultra-performance liquid chromatography-tandem mass spectrometric method for the determination of tetrandrine,fangchinoline,and cyclanoline in rat plasma and to investigate their pharmacokinetics after oral administration of Stephaniae Tetrandrae Radix extracts.Methods:Sample pretreatment involved methanol pretreatment and liquid–liquid extraction of ethyl acetate from plasma with methanol.Tramadol was used as the internal standard.The analysis was performed using an high strength silica T3 column(100 mm×2.1 mm,1.8μm)and a gradient elution method consisting of mobile phase solution A(0.1%formic acid in water)and B(acetonitrile)at a flow rate of 0.4 mL/min.The detection was performed using a triple quadrupole tandem mass spectrometer in the multiple reaction monitoring mode and using an electrospray ionization source in the positive ionization mode.Results:High efficiency was achieved with an analysis time of 4 min/sample.The calibration curve linear in the concentration range of 1250 ng/ml(R^(2)≥0.9900)and the lower limit of quantification is 1 ng/ml.The intraday and interday precision(relative standard deviation)values were lower than 9.4.Accuracy(relative error)was within 10.3%at all three quality control levels.Conclusions:This method was successfully applied in pharmacokinetics of tetrandrine,fangchinoline,and cyclanoline in rats after oral administration of Stephaniae Tetrandrae Radix extracts.The maximum plasma concentration(C_(max))of tetrandrine,fangchinoline,and cyclanoline was 124.71±16.08,84.56±3.28,and 57.61±6.26 ng/mL,respectively.The time to reach C_(max)was 10.39±3.04 for tetrandrine,10.17±3.04 for fangchinoline,and 6.40±3.16 for cyclanoline.The pharmacokinetic results might help further guide the clinical application of Stephaniae Tetrandrae Radix.
基金supported by the National Science & Technology Major Project (2009ZX09301-14)the National Natural Science Foundation of China (90817103,20775055 & 30973672)+1 种基金the Startup Funding for ZC’s Luojia Chair Professorship of Wuhan University (306276216 & 306271159)the Fundamental Research Funds for the Central Universities
文摘A new liquid chromatography-mass spectrometry method for the determination of carbamazepine,clonazepam,alprazolam,estazolam and phenytoin in human plasma has been developed by using diazepam as an internal standard.Chromatographic separation was performed on a Zorbax SB-C18 column(30 mm × 2.1 mm,3.5 ?m) with a mobile phase consisting of methanol and aqueous 25 mM ammonium acetate using gradient elution.A diethyl ether extraction method was used for the extraction of five anti-epilepsy drugs.The final extract was injected for analysis by LC-MS/MS.The method was validated within the concentration range of 50-5000 ng mL-1 for five anti-epilepsy drugs.The precision of the assay(RSD%) was less than 10% at all concentration levels within the tested range.The method recoveries for all samples were more than 90%.The results indicate that the method is specific,sensitive and accurate,and suitable to study the pharmacokinetics,to adjust the dosage for individual administration,and to monitor the drug-concentration and drug abuse of the five anti-epilepsy drugs.
文摘A sensitive, accurate and robust Liquid Chromatography Tandem Mass Spectrometry method has been developed and validated to measure voriconazole trough levels in human plasma. The plasma samples were mixed with fluconazole as an Internal Standard and directed to protein precipitation and drug extraction. An aliquot of 1 μl was injected into the chromatographic system and separated by the Acquity BEH C18 column at a flow rate of 0.30 ml/min in a gradient mobile phase consisting of acetonitrile, Ultrapure water (UPW), methanol and formic acid. Voriconazole was detected by a Triple Quadrupole Detector (TQD) operating on Multiple Reaction Monitoring (MRM) and a positive ion mode Electrospray ionization (ESI) Q1 mass: 350.1 m/z, Q3 mass: 281.1 m/z. Method linearity of the calibration curve (0.10 - 8.00 μg/ml) indicated a correlation coefficient r ≥ 0.99. The intra and inter-assay accuracy was within 85% - 115% and the intra and inter-assay precision was ≤5.76%. Voriconazole recovery percentage was between 97.69 - 119.62%. The method was successively applied in routine voriconazole TDM.
基金supported by National Key Research and Development Program of China(2019YFC1606400)Science and Technology Project of State Administration for Market Regulation(2021MK023)+1 种基金Hebei Province High-level Talent Funding Program(A201901008)Research Project of Hebei Administration for Market Regulation(2020ZD12)。
文摘The aim of this work was to develop a liquid chromatography-tandem mass spectrometry method for the determination of milk allergen and egg allergen in food products.Signature peptides GGLEPINFQTAADQAR,VGINYWLAHK,VLVLDTDYK,FFVAPFPEVFGK,and NAVPITPTLNR were confirmed and synthesized as the quantitative peptide of ovalbumin,α-lactalbumin,β-lactoglobulin,α_(S1)-casein andα_(S2)-casein,the relative isotope-labeled internal standards were used in the quantitative analysis.Linear range was in the range of0.5-5000.0 nmol/L for egg and milk allergen in bread,cake,cookie,rice crust and wheat flour samples with free from egg and milk,the limits of detection of milk allergens and egg allergen were in the range between0.94 mg/100 g and 56.71 mg/100 g,limits of quantification of milk allergens and egg allergen were in the range between 2.36 mg/100 g and 141.78 mg/100 g.The recoveries ranged from 76.7%to 122.8%,the relative standard deviations were in the range of 1.60%-15.60%.The developed method has been successfully used for the detection of egg and milk allergen in various food samples.
基金Project(51178321)supported by the National Natural Science Foundation of ChinaProject(2012ZX07403-001)supported by the National Science and Technology Major Project,ChinaProject(20120072110050)supported by the Research Fund for the Doctoral Program of Higher Education of China
文摘A simple and rapid technique based on liquid-liquid extraction coupled to gas chromatography-mass spectrometric detection(LLE-GC-MS) was developed for analysis of taste and odour compound β-ionone in water. Instrument parameters including programmed oven temperature, injection temperature and ion source temperature were evaluated and optimized. Effects of extraction time, ionic strength and p H on the detection efficiency were investigated and optimum conditions were 8 min of extraction time, without Na Cl addition at p H=9. Good linearity(R2=0.9997) was obtained when the linear range was 10-500 μg/L. The recoveries of β-ionone in ultrapure water and tap water samples were 88%-95% and 110%-114%, respectively. The relative standard deviations(RSD) were less than 10%. The method detection limit(MDL) and rejection quality level(RQL) were achieved at1.98 μg/L and 6.53 μg/L, respectively. LLE-GC-MS was demonstrated to be a rapid and convenient method for the determination ofβ-ionone in water samples.
基金Supported by The Fourth Batch of High-end Talent Project in Hebei ProvinceTangshan Science and Technology Entrepreneurship and Innovation Leading Talent Project(21130243A).
文摘[Objectives]A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was established for the determination of 14β-receptor agonist residues in mutton.[Methods]Samples were hydrolyzed byβ-glucuronidase and extracted with 5%acetic acid-acetonitrile(1:99,V/V)solution.An Eclipse plus C 18 column was used for separation,and the MRM mode was used for qualitative analysis,and the external standard method was used for quantitative analysis of matrix standard solutions.[Results]Under the optimal conditions,the retention time of the 14 kinds ofβ-receptor agonists ranged from 1.0 to 9.5 min.When the mass concentration was in the range of 0.05-0.50μg/ml,the linear relationship ofβ-receptor agonists was good,with correlation coefficients(r)≥0.9992.The detection limits of the method were in the range of 0.04-0.87μg/kg,and the quantitative limits were in the range of 0.35-1.86μg/kg.The average recovery values were in the range of 82.8%-108.9%,with RSDs(n=6)in the range of 1.9%-6.7%.[Conclusions]The method is simple,sensitive,reproducible,accurate,and can be used for simultaneous determination of the 14 kinds ofβ-receptor agonist residues in mutton.