Modernization of Chinese herbal compound and the high performance liquid chromatography tandem mass spectrometry (HPLC-MS)

Chinese herbal compound is playing an important role on curing human diseases.And it has been a trend that Chinese herbal compound is being used all over the world in 21 century.However,our Chinese herbal compound is facing serious challenge for the lack of canonical system of quality criterion for Chinese herbal compound so it has been a urgent problem to set up the quality control standards and reveal therapeutic basis of Chinese herbal compound.In order to give full play to the advantages of Chinese herbal compound,modern scientific and technological is used to research of Chinese herbal compound,especially the high performance liquid chromatography tandem mass spectrometry(HPLC-MS),because it is high sensitive,rapid,and obtain more information.It is very necessary that HPLC-MS is uesed to elucidate the effective components of basic substances of Chinese Herbal Compound,and endow traditional Chinese medicine with modern scientific connotation.

Simultaneous Determination of 14 β-Receptor Agonists Residues in Mutton by High Performance Liquid Chromatography-Tandem Mass Spectrometry (HPLC-MS/MS)

[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.

Determination of Sodium Pentachlorophenoxide Residues in Animal-derived Foods by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry (UPLC-MS/MS)

[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.

Ultra-soft Desorption Assisted Mass Spectrometry using Picosecond Infrared Laser for the Detection of lons in the Liquid Surface

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.

Analysis of ganciclovir and its related substances using high performance liquid chromatography and liquid chromatography-mass spectrometry methods

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.

Chemical Components of Achyranthes bidentata Leaves by Ultra High Performance Liquid Chromatography-Mass Spectrometry

[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.

Determination of Veterinary Drug Residues in Animal-derived Foods by Liquid Chromatography-Mass Spectrometry

[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.

A Validated Liquid Chromatography-Mass Spectrometry Method for the Detection and Quantification of Oxidative Metabolites of 2,2',4,4'-Tetrabromodiphenyl Ether in Rat Hepatic Microsomes

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.

Effect of pediatric tuina on hypothalamic metabolites in young rabbits using liquid chromatography-mass spectrometry

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.

CO₂Absorption Solvent Degradation Compound Identification Using Liquid Chromatography-Mass Spectrometry Quadrapole-Time of Flight (LCMSQTOF)

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 CO2 adsorption, within reasonable analysis time.

Liquid Chromatography-mass Spectrometry Analysis on Effect of Roughage Types on Liver Metabolic in Dairy Cows

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.

Novelties Filtration Theory of Liquid Chromatography-Mass Spectrometry in Volume Nanotube of Cotton Filament of Layers Woven Fabrics

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.

High Performance Liquid Chromatography-Electrospray Ionization-Mass Spectrometric Analysis of Bilobalide and Ginkgolides in Ginkgo biloba L. Leaves

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.

同位素内标稀释-UPLC-MS/MS法同时测定生活饮用水中5种消毒副产物和高氯酸盐

利用同位素稀释技术建立一种可同时测定生活饮用水中二氯乙酸、三氯乙酸、氯酸盐、亚氯酸盐和溴酸盐5种消毒副产物以及高氯酸盐的超高效液相色谱串联质谱(ID-UPLC-MS/MS)检测方法。样品过膜后加入同位素内标,采用Torus DEA色谱柱(100 mm×2.1 mm,1.7μm)分离,以0.5%氨水-1 mmol/L乙酸铵和乙腈为流动相洗脱,多反应监测(MRM)负模式(ESI-)测定,内标法定量。6种化合物线性相关系数r均大于0.990,检出限为1.5~2.1μg/L,定量限为5.0~7.0μg/L,应用该方法对399份水样进行测定,检出率为16.04%。该方法采用同位素内标稀释直接进样,分析速度快,灵敏度高,数据准确适用于饮用水国家标准(GB/T 5750.5—2023和GB/T 5750.10—2023)检测限值的要求。

Determination of penehyclidine hydrochloride in beagle dog plasma by liquid chromatography-electrospray ionization mass spectrometry and the pharmacokinetic study

To develop a fast and sensitive liquid chromatography-mass spectrometry method for the determination of penehyclidine hydrochloride （PH） in beagle dog plasma. PH and diphenhydramine hydrochloride （internal standard, IS） were extracted with a solvent mixture of petroleum ether-ethyl ether （7：3）. Chromatographic separation was achieved on a reversed-phase Eclipse XDB-C18 column （4.6 mm × 150 mm, 5 um） using the eluent of methanol-water （5 mmol/L ammonium acetate） （90：10, v/v, pH 5.8） as mobile phase. The electrospray ionization source was set at the positive multiple reaction monitoring （MRM） mode. This method involved the use of the [M＋H]^＋ ions of PH and diphenhydramine hydrochloride at m/z 316.4- 128.2 and m/z 256.4-167.2. The calibration curve was linear in the range of 1-1000 ng/mL with a correlation coefficient of 0.9988. The lower limit of quantification was 0.05 ng/mL. The precision, accuracy and recovery of the method were acceptable. Following intravenous injection admires＇ tration at doses of 0.5, 1 and 5 mg/kg PH, the main pharmacokinetic parameters were as the followings, t1/2a 0.33 h, t1/2β 2.44 1% tmax 0.058 1% AUC and Cmax exhibited a linear increase along with the increase of dose. The two-compartment model fit the three dose groups. This method was sensitive, accurate and fast for the determination of concentration of PH in beagle dog plasma. It could be used in pharmacokinetic studies of PH.

基于UPLC-MS/MS的有机栽培与常规栽培蔬菜差异代谢物分析

为明确有机栽培与常规栽培蔬菜的初生代谢产物及其代谢途径的差异,采用超高效液相色谱串联质谱(UPLC-MS/MS)检测技术对有机与常规栽培条件下大白菜、叶用莴苣与普通白菜(青梗菜)的叶片,以及辣椒与黄瓜的果实初生代谢物进行研究分析。结果表明:从有机栽培与常规栽培蔬菜叶片及果实中共鉴定出12类296种代谢产物,差异代谢物质主要包括异绿原酸A、对-羟基苯乙酸、对-香豆醇、阿魏酸、阿魏酰苹果酸、3-羟基-4-异丙基苯甲基乙醇-3-葡萄糖苷、新绿原酸等酚酸类物质,腺苷5’-单磷酸等核苷酸及其衍生物,(S)-2-(4-氨基丁酰胺基)-3-(1-甲基-1H-咪唑-5-基)丙醇、4-乙酰氨基丁酸等有机酸,以及N-苯乙酰基-L-谷氨酰胺等氨基酸及其衍生物。差异代谢产物以赖氨酸生物合成、赖氨酸降解、类黄酮的生物合成、半胱氨酸和蛋氨酸代谢等4条通路富集显著。有机栽培与常规栽培蔬菜叶片及果实营养品质和感官品质的不同很可能是这些差异性代谢产物共同作用的结果。

Determination of Ten Kinds of Alpha-2 Agonists Residues in Animal Derived Food by UHPLC-Triple Quadrupole/Composite Linear Ion Trap Mass Spectrometry

[Objectives]The paper was to establish an ultra high performance liquid chromatography-quadrupole/linear ion trap complex mass spectrometry for the determination of 10 kinds ofα2-receptor agonists in animal derived food.[Methods]The samples were extracted with sodium carbonate buffer solution and ethyl acetate,and analyzed by mass spectrometry after solid phase extraction and high performance liquid chromatography separation.[Results]Ten kinds ofα2-receptor agonists showed a good linear relationship in the range of 1-100μg/mL,with the average recovery of over 69%and the relative standard deviation less than 8.32%.The detection limit of 10 kinds of α_(2)-receptor agonists was up to 1μg/kg.[Conclusions]The method has good selectivity and strong anti-interference ability,and can meet the requirements of 10 kinds ofα2-receptor agonists residues in animal derived food.

Determination of urine catecholamines and metanephrines by reversed-phase liquid chromatography-tandem mass spectrometry

The measurement of urine catecholamine and metanephrine concentrations is important for biochemical screening and diagnosis of pheochromocytoma.The goal of this work was to develop a simple liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for determining catecholamines and metanephrines in urine to replace an existing liquid chromatographic method using electrochemical detection.Urine samples were prepared using Oasis weak-cation-exchange cartridges.The eluate was analyzed on an Agilent ZORBAX Eclipse Plus Phenyl-Hexyl column in 3 min.Adrenaline,noradrenaline,dopamine,metanephrine,normetanephrine,and their deuterated internal standards were monitored in positive electrospray ionization mode by multiple reaction monitoring(MRM).No evidence of ion suppression was observed.The assay was linear up to 5μmol/L for adrenaline,5μmol/L for noradrenaline,6.1μmol/L for dopamine,5.6μmol/L for metanephrine,and 34.6μmol/L for normetanephrine,with lower limits of quantification of 5,5,12,6 and 7nmol/L,respectively.The intra-day and inter-day precisions for all analytes ranged from 0.59%to 4.64%and1.98%to 4.80%,respectively.External quality assurance samples were assayed and showed excellent agreement with the target values.This simple method provides an improved assay for determining urine catecholamines and metanephrines.

Detection of 36 antibiotics in coastal waters using high performance liquid chromatography-tandem mass spectrometry

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

Offline two-dimensional liquid chromatography coupled with ion mobility-quadrupole time-of-flight mass spectrometry enabling fourdimensional separation and characterization of the multicomponents from white ginseng and red ginseng

Inherent complexity of plant metabolites necessitates the use of multi-dimensional information to accomplish comprehensive profiling and confirmative identification.A dimension-enhanced strategy,by offline two-dimensional liquid chromatography/ion mobility-quadrupole time-of-flight mass spectrometry(2 D-LC/IM-QTOF-MS)enabling four-dimensional separations(2 D-LC,IM,and MS),is proposed.In combination with in-house database-driven automated peak annotation,this strategy was utilized to characterize ginsenosides simultaneously from white ginseng(WG)and red ginseng(RG).An offline 2 DLC system configuring an Xbridge Amide column and an HSS T3 column showed orthogonality 0.76 in the resolution of ginsenosides.Ginsenoside analysis was performed by data-independent high-definition MSE(HDMSE)in the negative ESI mode on a Vion?IMS-QTOF hybrid high-resolution mass spectrometer,which could better resolve ginsenosides than MSEand directly give the CCS information.An in-house ginsenoside database recording 504 known ginsenosides and 58 reference compounds,was established to assist the identification of ginsenosides.Streamlined workflows,by applying UNIFI?to automatedly annotate the HDMSEdata,were proposed.We could separate and characterize 323 ginsenosides(including 286 from WG and 306 from RG),and 125 thereof may have not been isolated from the Panax genus.The established 2 D-LC/IM-QTOF-HDMSEapproach could also act as a magnifier to probe differentiated components between WG and RG.Compared with conventional approaches,this dimensionenhanced strategy could better resolve coeluting herbal components and more efficiently,more reliably identify the multicomponents,which,we believe,offers more possibilities for the systematic exposure and confirmative identification of plant metabolites.