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Simultaneous Determination of 14 β-Receptor Agonists Residues in Mutton by High Performance Liquid Chromatography-Tandem Mass Spectrometry (HPLC-MS/MS)
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作者 Zhe MENG Jianhua WANG +5 位作者 Bo LIU Yuhang GUO Haoshuang DONG Pingyang SHAN Dawei WANG Yajuan SONG 《Agricultural Biotechnology》 CAS 2023年第5期55-58,共4页
[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
关键词 MUTTON High performance liquid chromatography-tandem mass spectrometry β-receptor agonist RESIDUE
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Determination of Oleuropein in Cosmetics by Ultra Performance Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry
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作者 Pan Lijing Chen Weiwei Yuan Minjia 《China Detergent & Cosmetics》 CAS 2023年第4期30-36,共7页
An ultrahigh performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established to quickly and accurately determine the content of oleuropein in cosmetics.The samples were extracte... An ultrahigh performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established to quickly and accurately determine the content of oleuropein in cosmetics.The samples were extracted with methanol-aqueous solution,and the mobile phase with methanol-formic acid solution(0.1 mol/L)=40∶60 was separated by Agilent ZORBAX Eclipse Plus C18(2.1 mm×50 mm×1.8μm-Micron)column temperature 30℃,flow rate 0.3 mL/min.The MS end was detected by electrospray negative mode ionization(ESI-)and multiple reaction monitoring(MRM)mode.The results show a good linear relationship in the range of 0.002~5 mg/L,with a correlation coefficient R2 of 0.999,5.Method recovery range from 84.2%~107.6%and the relative standard deviation RSD is 5.8%.The detection time is 5 min,the detection limit is 0.000,6 mg/L,and the limit of quantification is 0.002 mg/L.This method has the advantages of convenient operation,low quantification limit,high precision and good repeatability,and is suitable for measuring the content of oleuropein in many kinds of cosmetics. 展开更多
关键词 ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS) OLEUROPEIN COSMETICS
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Detection of 36 antibiotics in coastal waters using high performance liquid chromatography-tandem mass spectrometry 被引量:13
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作者 那广水 顾佳 +4 位作者 葛林科 张蓬 王震 刘春阳 张琳 《Chinese Journal of Oceanology and Limnology》 SCIE CAS CSCD 2011年第5期1093-1102,共10页
Among pharmaceuticals and personal care products released into the aquatic environment, antibiotics are of particular concern, because of their ubiquity and health effects. Although scientists have recently paid more ... Among pharmaceuticals and personal care products released into the aquatic environment, antibiotics are of particular concern, because of their ubiquity and health effects. Although scientists have recently paid more attention to the threat of antibiotics to coastal ecosystems, researchers have often focused on relatively few antibiotics, because of the absence of suitable analytical methods. We have therefore developed a method for the rapid detection of 36 antibiotic residues in coastal waters, including tetracyclines (TCs), sulfanilamides (SAs), and quinolones (QLs). The method consists of solid-phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis, using electrospray ionization (ESI) in positive mode. The SPE was performed with Oasis HLB and Oasis MCX cartridges. Chromatographic separation on a Cr8 column was achieved using a binary eluent containing methanol and water with 0.1% formic acid. Typical recoveries of the analytes ranged from 67.4% to 109.3% at a fortification level of 100 ng/L. The precision of the method, calculated as relative standard deviation (RSD), was below 14.6% for all the compounds. The limits of detection (LODs) varied from 0.45 pg to 7.97 pg. The method was applied to detemaine the target analytes in coastal waters of the Yellow Sea in Liaoning, China. Among the tested antibiotics, 31 were found in coastal 'waters, with their concentrations between the LOD and 212.5 ng/L. These data indicate that this method is valid for analysis of antibiotics in coastal waters. The study first reports such a large number of antibiotics along the Yellow Sea coast of Liaoning, and should facilitate future comprehensive evaluation of antibiotics in coastal ecosystems 展开更多
关键词 ANTIBIOTICS high performance liquid chromatography-tandem mass spectrometry SOLID-PHASEEXTRACTION coastal waters
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Simultaneous Determination of Bisphenols and Alkylphenols in Water by Solid Phase Extraction and Ultra Performance Liquid Chromatography-tandem Mass Spectrometry 被引量:4
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作者 SHAN Xiao Mei SHEN Deng Hui +2 位作者 WANG Bing Shuang LU Bei Bei HUANG Fa Yuan 《Biomedical and Environmental Sciences》 SCIE CAS CSCD 2014年第6期471-474,共4页
To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry ... To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry (UPLC/MS/MS). The water samples were extracted and condensed with solid-phase extraction (SPE) using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%. 展开更多
关键词 UPLC BPA Simultaneous Determination of Bisphenols and Alkylphenols in Water by Solid Phase Extraction and Ultra performance liquid chromatography-tandem mass spectrometry mass
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Determination of Steroid Hormone Residues in Fish Tissues Using Gel Permeation Chromatography and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry 被引量:3
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作者 LI Peipei YAN Zhongyong +3 位作者 SUN Xiumei CHEN Si CHEN Yin ZHANG Xiaojun 《Journal of Ocean University of China》 SCIE CAS CSCD 2018年第5期1171-1177,共7页
A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 s... A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 steroid hormones were extracted from the tissues with diethyl ether.Differing from other common purification methods,the extract solutions were cleaned by gel permeation chromatography(GPC) using ethyl acetate-cyclohexane solution(1:1,v/v) as the mobile phase.The separation of target compounds was carried out by a BEH C18 column and a gradient elution consisting of acetonitrile and 0.2% aqueous formic acid(v/v).The compounds were detected under the multiple reaction monitoring(MRM) mode and quantified with external standard method.This method was validated with respect to linearity,specificity,accuracy and precision.A linearity with correlation coefficient larger than 0.995 was achieved in the range of 0.5 to 50 ng m L^(-1).The average recoveries at the spiked levels of 1.0,5.0,and 10.0 μg kg^(–1) varied between 81.7% and 90.8%,with the relative standard deviations(n=5) ranged from 3.50% to 10.0%.The limit of quantification(LOQ) for 8 steroid hormones ranged from 0.2 to 1.5 μg kg^(-1).It was concluded that this method can be successfully applied for the determination of 8 steroid hormones in complicated matrices including high-fat fish tissues. 展开更多
关键词 ultra performance liquid chromatography-tandem mass spectrometry anabolic hormone gel permeation chromatography fish tissue
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Determination of Sulfadimidine in Royal Jelly by C_(18)-functionalized Magnetic Silica Nanoparticles Solid Phase Extraction-High Performance Liquid Chromatography-Tandem Mass Spectrometry
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作者 李金峰 李颖 +3 位作者 蒋原 薛峰 戴劲 朱海 《Agricultural Science & Technology》 CAS 2012年第11期2278-2280,共3页
[Objective] This study aimed to develop a method of C_18-functionalized magnetic silica nanoparticles solid phase extraction-high performance liquid chro- matography-tandem mass spectrometry for the determination of s... [Objective] This study aimed to develop a method of C_18-functionalized magnetic silica nanoparticles solid phase extraction-high performance liquid chro- matography-tandem mass spectrometry for the determination of sulfadimidine in royal jelly. [Method] The royal jelly samples were pretreated by MCX SPE column and C_18-functionalized magnetic silica nanoparticles, and the purified samples were de- tected by HPLC-MS/MS. [Result] The detection method showed a good linear rela- tionship in the range of 5-80 ugkg (r=0.993 1). The recovery ranges were between 93%- 104% with the relative standard deviations (RSD) below 11.3%. [Conclusion] Combined with automation equipment, the method is simple, fast, time-saving, and easy to real- ize the automation of sulfadimidine in the royal jelly samples before determination. 展开更多
关键词 Solid phase extraction Magnetic silica nanoparticles Sulfadimidine Highperformance liquid chromatography-tandem mass spectrometry
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Uncertainty Evaluation of Determination of Microcystin MC-LR in Environmental Samples by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry 被引量:1
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作者 Zhao Bin Zhang Min Zhang Fuhai 《Meteorological and Environmental Research》 CAS 2016年第6期54-57,共4页
To assess uncertainty of determination of MC-LR in environmental samples by solid phase extraction- ultra performance liquid chromatography- tandem mass spectrometry,the sources of the uncertainty were evaluated first... To assess uncertainty of determination of MC-LR in environmental samples by solid phase extraction- ultra performance liquid chromatography- tandem mass spectrometry,the sources of the uncertainty were evaluated firstly,and the expanded uncertainty was calculated finally.The results show that when MC-LR concentration in the water samples was 0.50 μg/L,the expanded uncertainty was 0.00628 μg/L(k=2). 展开更多
关键词 Uncertainty SOLID phase extraction Ultra performance liquid CHROMATOGRAPHY TANDEM mass spectrometry MICROCYSTIN MC-LR China
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High Performance Liquid Chromatography-Electrospray Ionization-Mass Spectrometric Analysis of Bilobalide and Ginkgolides in Ginkgo biloba L. Leaves 被引量:1
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作者 卢定强 韦萍 +1 位作者 欧阳平凯 陈钧 《Journal of Chinese Pharmaceutical Sciences》 CAS 2002年第2期26-30,共5页
The ginkgo terpenoids including bilobalide and ginkgolides are the main pharmaceutical components in the leaves or extracts of Ginkgo biloba L. In this paper, the analysis of bilobalide and ginkgolides in leaves of Gi... The ginkgo terpenoids including bilobalide and ginkgolides are the main pharmaceutical components in the leaves or extracts of Ginkgo biloba L. In this paper, the analysis of bilobalide and ginkgolides in leaves of Ginkgo biloba L. by high performance liquid chromatography (HPLC)-electrospray ionization (ESI)-mass spectrometry (MS) was carried out. The separation was performed on Inertsil ODS3 column with methanol-water (36:64) as mobile phase, with 1 mL·min -1 of flow rate at 35℃. Then the mass spectrum analysis was conducted by ZMD micromass electrospray ionization (ESI)-mass spectrometer (MS). The HPLC total ion chromatogram and selected ion chromatogram (with 325, 407, 423, 439 of m/z) of the sample and ESI-/MS mass spectra of the peaks in the chromatograms were obtained. So bilobalide, ginkgolide A, B, C and J in Ginkgo biloba L. leaves were identified. The method is easy and rapid, with a good accuracy. 展开更多
关键词 High performance liquid chromatography Electrospray ionization mass spectrometry Ginkgo terpene lactones
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Determination of thyreostats in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry
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作者 Lech RODZIEWICZ Jolanta MASLOWIECKA +1 位作者 Anna SADOWSKA Halina CAR 《色谱》 CAS CSCD 北大核心 2017年第10期1048-1054,共7页
Five thyreostats(TSs),namely tapazole,thiouracil,methylthiouracil,propylthiouracil,and phenylthiouracil,were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC... Five thyreostats(TSs),namely tapazole,thiouracil,methylthiouracil,propylthiouracil,and phenylthiouracil,were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)in positive electrospray ionization mode.Extraction and clean-up were achieved using a ChemElut cartridge with tert-butyl methyl ether,without a derivatization step.Separation was achieved on an Acquity UPLC SS T3 column.The mobile phase was acetonitrile and water containing 0.2%(v/v)formic acid.The mass spectrometer was operated in multiple reaction monitoring mode.Urine samples were spiked with TS solution at levels corresponding to 5,10,15,and 20μg/L.The accuracy(internal standard corrected)ranged from 92%to 107%,with a repeatability precision(relative standard deviation,RSD)less than 15%for all five analytes.The RSDs within-laboratory reproducibility was less than 26%.The decision limits(CCα)and detection capabilities(CCβ)were obtained from a calibration curve and were in the ranges of 3.1-6.1μg/L and 4.0-7.4μg/L,respectively.The CCαand CCβvalues were below the recommended concentration,which was set at 10μg/L.The results show that the described method is suitable for the direct detection of TSs in bovine urine.This method can also be used to determine TSs in porcine urine. 展开更多
关键词 ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) thyreostats (TSs) URINE
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Rapid Determination of Three Kinds of Microcystins in Environmental Water Samples by Disk SPE-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
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作者 Zhao Bin Zhang Min Zhang Fuhai 《Meteorological and Environmental Research》 CAS 2016年第5期62-64,68,共4页
A method of rapidly detecting three kinds of microcystins( MCs) in environmental water samples by using disk SPE- ultra high performance liquid chromatography- tandem mass spectrometry( UPLC- MS / MS) was established.... A method of rapidly detecting three kinds of microcystins( MCs) in environmental water samples by using disk SPE- ultra high performance liquid chromatography- tandem mass spectrometry( UPLC- MS / MS) was established. Firstly,environmental water samples were extracted by disk SPE column( C_(18)),and three kinds of MCs were separated by Waters BEH C_(18) chromatographic column with acetonitrile- 0. 2% formic acid solution as the mobile phase. After the gradient elution separation,the external standard method was used for quantitative and qualitative analysis under MRM of UPLC- MS / MS. The results showed that the three kinds of MCs in the range of 0. 05- 10 μg / L showed good linear relation,and the correlation coefficients were higher than 0. 999 4,while the method detection limit was 0. 04 ng / L. Under 0. 1,1,and 5 μg / L standard addition for the same environmental sample,the average recovery was 82. 8%- 108. 8%,and the relative standard deviation of determination results was2. 1%- 10. 1%( n = 6). This method is rapid,sensitive and accurate,so it can be effectively applied in the monitoring of MCs in environmental water samples. 展开更多
关键词 Disk SOLID-PHASE extraction COLUMN Ultra performance liquid chromatography-tandem mass spectrometry Environmental water sample MICROCYSTINS Lake Chao China
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Determination of Sodium Pentachlorophenoxide Residues in Animal-derived Foods by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry (UPLC-MS/MS)
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作者 Chengmei WANG Chunxia CHENG +2 位作者 Guixia YANG Susu ZHANG Xuan QIAN 《Agricultural Biotechnology》 CAS 2022年第2期99-101,105,共4页
[Objectives]This study was conducted to establish an ultra-high performance liquid chromatography-tandem mass spectrometry for the rapid extraction of sodium pentachlorophenoxide from animal-derived food.[Methods]The ... [Objectives]This study was conducted to establish an ultra-high performance liquid chromatography-tandem mass spectrometry for the rapid extraction of sodium pentachlorophenoxide from animal-derived food.[Methods]The samples were extracted with an acetonitrile water solution(8∶2),0.1 mol/L hydrochloric acid and a purification extraction bag with shaking.Centrifugation was performed to obtain supernatants,which were added to purification tubes containing PSA and C_(18) for purification,and then filtered with membranes for determination.Each test solution was separated by a ZORBAX Eclipse plus C_(18) column with acetonitrile and 5 mmol/L ammonium acetate as mobile phases,and determined with electrospray ionization and multiple reaction monitoring.[Results]The method had good linearity in the concentration range of 1.0-50 ng/ml,and the correlation coefficient was 0.9997.The limit of detection was 0.25μg/kg and the limit of quantification was 0.75μg/kg.The recovery was between 87.4%and 112.5%,and the RSD%was between 0.5%and 10.0%.[Conclusions]The method has simple operation and high sensitivity,and is suitable for trace detection of sodium pentachlorophenoxide in large quantities of animal-derived food. 展开更多
关键词 Sodium pentachlorophenoxide Ultra-high performance liquid chromatography-tandem mass spectrometry Animal-derived food Trace analysis
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An Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry Method for the Quantification of Vancomycin Requiring Only 2 μL of Rabbit Serum
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作者 Veronika Schmitt Andras Szeitz +1 位作者 Tara L.Klassen Urs O.Hafeli 《American Journal of Analytical Chemistry》 2017年第9期553-563,共11页
A highly sensitive ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed for the quantification of vancomycin (VAN) in low volumes of rabbit serum. For each analysis,... A highly sensitive ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed for the quantification of vancomycin (VAN) in low volumes of rabbit serum. For each analysis, 2 μL rabbit serum was precipitated with methanol that contained the internal standard teicoplanin (TEI). The supernatant was transferred into a 384 well-plate, diluted with water, covered with a pierceable silicone mat and 5 μL was analyzed in positive ionization mode. The UHPLC-MS/MS consisted of an Agilent 1290 Infinity UHPLC system connected to an AB Sciex QTrap&reg;5500 hybrid linear ion-trap triple quadrupole mass spectrometer equipped with a Turbo Spray source. Chromatographic separation was achieved using a Waters Acquity UPLC BEH C18 (1.7 μm, 2.1 mm × 100 mm) column, a VanGuard (1.7 μm, 2.1 × 5 mm) guard column and a mobile phase of water and methanol both containing 5 mM ammonium acetate with 0.1% formic acid. VAN was quantified with multiple reaction monitoring using the transitions of m/z 725.5/144.2, and TEI was monitored at m/z 940.6/316.4. The accuracy, precision, linearity, range and lower limit of quantification (LLOQ) were determined. The accuracy was ≤9.93% and the precision was ≤10.6%. The range was established as 0.1 to 40 μg·mL-1. The LLOQ was 0.1 μg·mL-1 VAN requiring 2 μL of sample with an accuracy of -20.2% and precision of 8.39%. The method was applied successfully to determine the VAN concentrations in rabbit serum after the i.v. administration of VAN via implanted ear catheters. 展开更多
关键词 Ultra-High performance liquid chromatography-tandem mass spectrometry VANCOMYCIN RABBIT SERUM PHARMACOKINETICS
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Determination of egg and milk allergen in food products by liquid chromatography-tandem mass spectrometry based on signature peptides and isotope-labeled internal standard
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作者 Sufang Fan Junmei Ma +4 位作者 Zhuo Liu Yawei Ning Meicong Cao Qiang Li Yan Zhang 《Food Science and Human Wellness》 SCIE CSCD 2023年第3期728-736,共9页
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
关键词 liquid chromatography-tandem mass spectrometry Egg and milk allergen Signature peptides Isotope-labeled internal standards
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Bio-analytical method development and validation of Rasagiline by high performance liquid chromatography tandem mass spectrometry detection and its application to pharmacokinetic study 被引量:2
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作者 Ravi Kumar Konda Babu Rao Chandu +1 位作者 B.R.Challa Chandrasekhar B.Kothapalli 《Journal of Pharmaceutical Analysis》 SCIE CAS 2012年第5期342-349,共8页
The most suitable bio-analytical method based on liquid liquid extraction has been developed and validated for quantification of Rasagiline in human plasma. Rasagiline-13C3 mesylate was used as an internal standard fo... The most suitable bio-analytical method based on liquid liquid extraction has been developed and validated for quantification of Rasagiline in human plasma. Rasagiline-13C3 mesylate was used as an internal standard for Rasagiline. Zorbax Eclipse Plus C18 (2.1 mm × 50 mm, 3.5 um) column provided chromatographic separation of analyte followed by detection with mass spectrometry. The method involved simple isocratic chromatographic condition and mass spectrometric detection in the positive ionization mode using an API-4000 system. The lotal run time was 3.0 min. The proposed method has been validated with the linear range of 5 12000 pg/mL for Rasagiline. The intra-run and inter-run precision values were within 1.3% 2.9% and 1.6% 2.2% respectively for Rasagiline. The overall recovery for Rasagiline and Rasagiline-13C3 mesylate analog was 96.9% and 96.7% respectively. This validated method was successfully applied to the bioequivalence and pharmacokinetic study of human volunteers under fasting condition. 展开更多
关键词 High performance liquid chromatography mass spectrometry RASAGILINE liquid-liquid extraction
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Analysis of ganciclovir and its related substances using high performance liquid chromatography and liquid chromatography-mass spectrometry methods 被引量:1
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作者 Cheng-Ping Li1,2,Mao Mao1,Lan-Jun Zheng1,Wei-Guang Shan11.College of Pharmaceutical Sciences,Zhejiang University of Technology,Hangzhou 310032 2.College of Biology and Environment Engineering,Zhejiang Shuren University,Hangzhou 310015,China 《Journal of Pharmaceutical Analysis》 SCIE CAS 2010年第4期218-222,共5页
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
关键词 GANCICLOVIR related substances high performance liquid chromatography high performance liquid chromatography/mass spectrometry
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Comparison of pharmacokinetics of different oral Panax notoginseng saponins using ultra-high performance liquid mass spectrometry 被引量:2
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作者 Huichao Wu Huimin Liu +3 位作者 Shouyin Du Jie Bai Yang Lu Lin Zhang 《Journal of Traditional Chinese Medical Sciences》 2021年第1期90-98,共9页
Objective:To discuss and compare the plasma pharmacokinetics after three oral Panax notoginseng saponin(PNS)administrations in beagle dogs.PNS is the main active ingredient of the traditional Chinese medicine(TCM)Pana... Objective:To discuss and compare the plasma pharmacokinetics after three oral Panax notoginseng saponin(PNS)administrations in beagle dogs.PNS is the main active ingredient of the traditional Chinese medicine(TCM)Panax notoginseng.Although its outstanding therapeutic efficacy has been demonstrated by various researchers,its broader application is restricted by the low bioavailability of PNS.Methods:An ultra-high performance liquid chromatographyetandem mass spectrometry(UPLC-MS/MS)method for the simultaneous quantification of notoginsenoside R1,ginsenoside Rg1,ginsenoside Rb1,ginsenoside Rd,and ginsenoside Re in beagle dog plasma was developed and validated.The plasma samples were subjected to liquideliquid extraction with acetone and methanol,and separated on an ACQUITY C18 column(100×2.1 mm ID,1.7 mm)using acetonitrile and water as the mobile phase with a run time of 4.5 min.Results:The analytes were detected without interference in Selected Reaction Monitoring mode with positive electrospray ionization.The validated method was successfully used in comparative pharmacokinetic studies of the five saponins in beagle dogs after oral administration of three PNS preparations.Blood samples were collected up to 192 h after administration and pharmacokinetic parameters were calculated using DAS 3.20 and SPSS 17.0.The AUC_(0-t)values of Re and R1 were significantly higher in soft capsules than in hard capsules.However,the AUC_(0-t)values between hard and soft capsules were not significantly different for the other three componentsdRb1,Rd and Rg1.Conclusion:Our intuitive analysis suggests that the bioavailability of PNS in soft capsules is greater than in hard capsules. 展开更多
关键词 Ultra-high performance liquid mass spectrometry Panax notoginseng saponin preparation Soft capsule Hard capsule Comparison of pharmacokinetics
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Metabolomic Studies Using High Performance Liquid Chromatography and Tandem Mass Spectrometry to Discover Quality Markers for Oriental Beauty (Dongfang Meiren) Tea 被引量:1
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作者 Yi-Hong Chen Yu-Hui Liu +1 位作者 Yi-Jhen Wu Chu-Chin Chen 《Food and Nutrition Sciences》 2014年第9期823-834,共12页
In this study, a high-performance liquid chromatograph and an electrospray ionization (ESI) triple quadrupole mass spectrometry (TQ MS) detector were used to scan Oriental Beauty tea of different grades and prices. Pr... In this study, a high-performance liquid chromatograph and an electrospray ionization (ESI) triple quadrupole mass spectrometry (TQ MS) detector were used to scan Oriental Beauty tea of different grades and prices. Principle component analysis (PCA) of the profiling data was performed for pattern recognition, clearly showing that the proposed MS profiling method was able to classify Oriental Beauty tea into different grades. The component mass ions primarily responsible for the separation were selected with high loading strength in the PCA for subsequent identification with tandem mass (MS/MS). Caffeine, citrate and salicylate were verified, whereas certain other compounds remained ambiguous. Regression analysis considering caffeine, citrate and salicylate showed a linear relationship between the prices of the Oriental Beauty tea with an adjusted R2 of 0.84. If all the selected marker ions (in addition to caffeine, citrate and salicylate) could have been identified and incorporated into regression analysis, a stronger relationship could have been confirmed. These results suggest that metabolomics can facilitate the determination of real markers in the quality control of Oriental Beauty tea, and may lead to the further application of metabolomics in other food quality controls. 展开更多
关键词 Dongfang Meiren High performance liquid Chromatography mass spectrometry Metabolic Profiling Metabolomics ORIENTAL BEAUTY QUALITY TEA
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Dimension-Enhanced Ultra-High Performance Liquid Chromatography/Ion Mobility-Quadrupole Time-of-Flight Mass Spectrometry Combined with Intelligent Peak Annotation for the Rapid Characterization of the Multiple Components from Seeds of Descurainia sophia 被引量:1
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作者 Simiao Wang Xue Li +7 位作者 Boxue Chen Shitong Li Jiali Wang Jing Wang Mingshuo Yang Xiaoyan Xu Hongda Wang Wenzhi Yang 《Phyton-International Journal of Experimental Botany》 SCIE 2022年第3期541-567,共27页
The complex composition of herbal metabolites necessitates the development of powerful analytical techniques aimed to identify the bioactive components.The seeds of Descurainia sophia(SDS)are utilized in China as a co... The complex composition of herbal metabolites necessitates the development of powerful analytical techniques aimed to identify the bioactive components.The seeds of Descurainia sophia(SDS)are utilized in China as a cough and asthma relieving agent.Herein,a dimension-enhanced integral approach,by combining ultra-high performance liquid chromatography/ion mobility-quadrupole time-of-flight mass spectrometry(UHPLC/IMQTOF-MS)and intelligent peak annotation,was developed to rapidly characterize the multicomponents from SDS.Good chromatographic separation was achieved within 38 min on a UPLC CSH C18(2.1×100 mm,1.7μm)column which was eluted by 0.1%formic acid in water(water phase)and acetonitrile(organic phase).Collision-induced dissociation-MS^(2)data were acquired by the data-independent high-definition MS^(E)(HDMS^(E))in both the negative and positive electrospray ionization modes.A major components knockout strategy was applied to improve the characterization of those minor ingredients by enhancing the injection volume.Moreover,a self-built chemistry library was established,which could be matched by the UNIFI software enabling automatic peak annotation of the obtained HDMS^(E)data.As a result of applying the intelligent peak annotation workflows and further confirmation process,a total of 53 compounds were identified or tentatively characterized from the SDS,including 29 flavonoids,one uridine derivative,four glucosides,one lignin,one phenolic compound,and 17 others.Notably,four-dimensional information related to the structure(e.g.,retention time,collision cross section,MS^(1)and MS^(2)data)was obtained for each component by the developed integral approach,and the results would greatly benefit the quality control of SDS. 展开更多
关键词 Descurainia sophia multicomponent characterization ultra-high performance liquid chromatography ion mobility/quadrupole time-of-flight mass spectrometry high-definition MS^(E) flavonoid
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Rapid Quantitative Determination of Isoprene Monomer in Living Taraxacum kok-saghyz by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry 被引量:1
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作者 Xiang Tong Guo Tianyang +5 位作者 Zhang Xi Chen Yunhan Dong Yiyang Zhang Jichuan Ma Qiang Zhang Liqun 《China Petroleum Processing & Petrochemical Technology》 SCIE CAS 2020年第2期30-36,共7页
Taraxacum kok-saghyz(TKS)is rich in natural rubber(NR),a natural organic macromolecular compound composed of cis-1,4-polyisoprene,and may become the second NR-bearing plant for biochemical engineering development.In t... Taraxacum kok-saghyz(TKS)is rich in natural rubber(NR),a natural organic macromolecular compound composed of cis-1,4-polyisoprene,and may become the second NR-bearing plant for biochemical engineering development.In this paper,a rapid and quantitative ultra-high performance liquid chromatography tandem mass spectrometry(UHPLCMS/MS)method was established for determination of macromolecular biosynthesis substrate(dimethylallyl pyrophosphate,DMAPP)and initiator(farnesyl pyrophosphate,FPP)contained in TKS.A Kromasil C18 chromatographic column was used for separation,and the multi-reaction monitoring mode(MRM)of triple quadrupole mass spectrometry was used for detection.Quantification was performed by external calibration method.The results showed that the limit of detection(LOD)and the limit of quantitation(LOQ)of DMAPP were 2.42μg/L and 7.26μg/L,respectively,and the LOQ and the LOD of FPP were 1.02μg/L and 3.05μg/L,respectively.At a concentration of 1—1000μg/L,both analytes had good determination coefficients(>0.999)of calibration curve.The recoveries of DMAPP and FPP were between 99.0%and 117.1%.In real samples detection,the contents of DMAPP and FPP in TKS samples were between 23.32—82.77μg/L and 12.03—85.67μg/L,respectively.Thus,this approach is a reliable method to quantify DMAPP and FPP in TKS. 展开更多
关键词 QUANTITATION Taraxacum kok-saghyz(TKS) ISOPRENOIDS ultra-high performance liquid chromatography tandem mass spectrometry(UHPLC-MS/MS) natural rubber(NR)
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Simultaneous Determination of Ultraviolet Absorbers and Antibacterial Agents in Textiles by Ultra-High Performance Liquid Chromatography/Orbitrap High Resolution Mass Spectrometry 被引量:1
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作者 Chengyun Wang Tangtang Xie +2 位作者 Rong Xu Junfeng Lin Lixia Li 《World Journal of Engineering and Technology》 2017年第1期1-18,共18页
This paper reported a new analytical method for the simultaneous determination of seven benzotriazole ultraviolet absorbers and seven antibacterial agents in textiles. After ultrasonic extraction for the textile sampl... This paper reported a new analytical method for the simultaneous determination of seven benzotriazole ultraviolet absorbers and seven antibacterial agents in textiles. After ultrasonic extraction for the textile samples in methanol, the solutions were analyzed by ultra-high performance liquid chromotagraphy/orbitrap high resolution mass spectrometry (UPLC/Orbitrap HRMS). It showed that a good chromatographic separation for these target compounds was achieved by a Hypersil GOLD column (100 mm × 2.1 mm × 1.9 μm) with a gradient elution of methanol and 0.1% aqueous formic acid solution (containing 0.5 mmol/L ammonium acetate). Triclosan and 4-chloro-3,5-dimethyl phenol (PCMX) were detected by the orbitrap HRMS in an electrospray ionization (ESI) negative mode while the other twelve target compounds were detected by orbitrap HRMS in ESI positive mode. Full scan experiment was performed over the range from m/z 100 to m/z 500. These target compounds were routinely detected with mass accuracy below 2 × 10-6 (2 ppm) at the optimized conditions. The results showed that the limits of detection (LODs) were in the range from 0.1 to 0.3 μg/kg. The blank samples were spiked at three levels and their average recoveries varied from 80.5% to 96.3% while the relative standard deviation (RSD) changed from 3.2% to 9.9%. The present method was also applied for the determination of those ultraviolet absorbers and antibacterial agents in the commercial textiles. 展开更多
关键词 Ultra-High performance liquid Chromatography/Orbitrap High Resolution mass spectrometry Benzotriazoleultraviolet ABSORBERS Isothiazolinone Tric-losan 4-Chloro-3 5-Dimethyl Phenol
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