Eighteen sex hormones in antler velvet were determined by high performance liquid chromatography tandem mass spectrometry.The solid phase extraction was applied to eliminating the matrix effect.The experimental condit...Eighteen sex hormones in antler velvet were determined by high performance liquid chromatography tandem mass spectrometry.The solid phase extraction was applied to eliminating the matrix effect.The experimental conditions were examined and optimized.Under the optimal conditions,the proposed method provides the good linearities and determination limits(0.2―1.0 μg/kg) of the analytes investigated.The recoveries ranging from 72.3% to 149.5% were obtained for the target analytes at two concentration levels.This method was applied to the determination of eighteen sex hormones in different kinds of antler velvet samples and the obtained results are satisfactory.The results indicate that the proposed method is suitable for the determination of sex hormones in antler velvet samples.展开更多
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
A reliable,selective and sensitive liquid chromatography tandem mass spectrometry method was developed and validated for the quantification of lamotrigine in human plasma using lamotrigine13C3,d3 as an internal standa...A reliable,selective and sensitive liquid chromatography tandem mass spectrometry method was developed and validated for the quantification of lamotrigine in human plasma using lamotrigine13C3,d3 as an internal standard.Analyte and internal standard were extracted from human plasma by solid-phase extraction and detected in positive ion mode by tandem mass spectrometry with electrospray ionization(ESI) interface.Chromatographic separation was performed on a Chromolith s SpeedROD;RP-18e column(50-4.6 mm i.d.) using acetonitrile:570.1 mM ammonium formate solution(90:10,v/v) as the mobile phase at a flow rate of 0.500 mL/min.The calibration curves were linear over the range of 5.02-1226.47 ng/mL with the lower limit of quantitation validated at 5.02 ng/mL.The analytes were found stable in human plasma through three freeze(-20℃)-thaw(ice-cold water bath) cycles and under storage on bench-top in ice-cold water bath for at least 6.8 h,and also in the mobile phase at 10℃ for at least 57h.The method has shown good reproducibility,as the intra-and inter-day precisions were within 3.0%,while the accuracies were within 76.0% of nominal values.The validated LC-MS/MS method was applied for the evaluation of pharmacokinetic and bioequivalence parameters of lamotrigine after an oral administration of 50mg lamotrigine tablet to thirty-two healthy adult male volunteers.展开更多
A rapid and sensitive liquid chromatography tandem mass spectrometry(LC-MS/MS) method has been developed and validated for the determination of moxifloxacin(MOXI) in human plasma. After a simple protein precipitation ...A rapid and sensitive liquid chromatography tandem mass spectrometry(LC-MS/MS) method has been developed and validated for the determination of moxifloxacin(MOXI) in human plasma. After a simple protein precipitation using acetonitrile, the post treatment samples were analysed on a C18 column interfaced with a Triple Quadropole Tandem Mass Spectrometer. Positive electrospray ionization was employed as the ionization source. The mobile phase consisted of 0.1% formic acid–acetonitrile(60:40, v/v). Ciprofloxacin(CIPRO) was used as an internal standard. The analyte and internal standard(CIPRO) were monitored in the multiple reaction monitoring mode(MRM). The mass transition ion-pair has been followed as m/z 402→358.2 for MOXI and 332→288.1 for CIPRO. The method was linear in the concentration range of 25–5000 ng/mL. The lower limit of quantification was 25 ng/mL. The intra- and inter-day precision(relative standard deviation) and accuracy(relative error) values were within 12.4%. Each plasma sample was analyzed within 3 min.展开更多
A rapid and high selective ultra-performance liquid chromatography(UPLC)with tandem mass spectrometry method for simultaneous determination of six compounds including albiflorin,paeoniflorin,picroside I,picroside II,s...A rapid and high selective ultra-performance liquid chromatography(UPLC)with tandem mass spectrometry method for simultaneous determination of six compounds including albiflorin,paeoniflorin,picroside I,picroside II,saikosaponin A,and saikosaponin D in rat plasma was developed and validated using butyl p-hydroxybenzoate as an internal standard.One-step direct protein precipitation with acetonitrile was used to extract the compounds from the rat plasma samples.Chromatographic separation was achieved using an ACQUITY UPLC BEH C18 column(100 mm×2.1 mm,1.7μm)at a flow rate of 0.4 m L/min,using gradient mode containing 0.1%formic acid in water and acetonitrile were used as the Mobile phase A and B.Electrospray ionization in negative ion mode and multiple reaction monitoring were used to identify and quantify active components.Calibration curves showed good linearity(R^2>0.9908)over a wide concentration range for all compounds.The intra-and interday precision(relative standard deviation)ranged 2.4%–7.0%and 2.6%–8.0%,respectively.The accuracy(relative error)was from-13.0%to 13.2%at all quality control levels.The recovery ranged from 81.1%to 92.5%.The validated method was successfully applied to pharmacokinetic study in rats after oral administration of Qing Gan-Shu Yu-Fang.The results show that one can draw a conclusion that these six active ingredients can be quickly absorbed and play a pharmacodynamic role rapidly in vivo.展开更多
Aspartame is a widely used sweetener, the long-term safety of which has been controversial ever since it was accepted for human consumption. It is unstable and can produce some harmful degradation products under certa...Aspartame is a widely used sweetener, the long-term safety of which has been controversial ever since it was accepted for human consumption. It is unstable and can produce some harmful degradation products under certain storage conditions. A high-performance liquid chromatography/tandem mass spectrometry method was developed for the simultaneous analysis of aspartame and its four degradation products, including aspartic acid, phenylalanine, aspartyl-phenylalanine and 5-benzyl-3,6- dioxo-2-piperazieacetic acid in water and in diet soft drinks. Aspartame and its four degradation products were quantified by a matrix matched external standard calibration curve with excellent correlation coefficients. The limits of detection were 0.16-5.8 μg/L, which exhibited higher sensitivity than common methods. This method was rapid, sensitive, specific and capable of eliminating matrix interferences. It was also applied to the study of the degradation of aspartame at various pH and temperatures. The results indicated that aspartame was partly degraded under strong acidic or basic conditions and the extent of degradation increased with increasing temperature.展开更多
A sensitive analytical method was developed to determine tetrodotoxin(TTX) in human plasma samples using protein precipitation, followed by ultra performance liquid chromatography(UPLC) analysis coupled with tande...A sensitive analytical method was developed to determine tetrodotoxin(TTX) in human plasma samples using protein precipitation, followed by ultra performance liquid chromatography(UPLC) analysis coupled with tandem mass spectrometry(MS/MS) using 11-deoxytetrodotoxin(11-deoxyTTX) as an internal standard. The plasma samples were prepared using protein precipitation prior to being analyzed by UPLC-MSfMS to identify TTX over a zwitterionic-hydrophilic interaction liquid chromatography column. The retention time values of TTX and 11-deoxyTTX were 4.12 and 3.67 min, respectively. TTX and 11-deoxyTTX were monitored and quantitated on the basis of their ion transitions for their respective precursor ions to their product ions(i.e., m/z 320.0→162. l for TTX and m/z 304.0→176.0 for 11-deoxyTTX) in the multiple reaction-monitoring mode. The lower limit of quantification of this method was determined to be 0.0199 ug/mL. This method showed good linearity for plasma samples that contained TTX concentrations in the range of 0.0199--1.99 ng/mL. The specificity, precision, accuracy, matrix effect, and stability characteristics of this method were also examined. The intra-assay precision and accuracy ranged from 1.89% to 6.00% and from 92.21% to 100.00%, whereas the inter-assay precision and accuracy ranged from 0.64% to 7.75% and from 99.38% to 101.26%, respectively. This new method therefore represents a rapid, accurate, reliable, and highly sensitive method for the qualitative and quantitative analyses of a trace amount of TTX in human plasma samples.展开更多
Curcumin,a safe natural yellow pigment with a wide range of pharmacological activities,is used both in herbal drugs and as a food coloring agents.Studies have shown that curcumin would suffer from extensive metabolism...Curcumin,a safe natural yellow pigment with a wide range of pharmacological activities,is used both in herbal drugs and as a food coloring agents.Studies have shown that curcumin would suffer from extensive metabolism in vivoand the predominant metabolic pathways are reduction and conjugation.In order to comprehensively study the metabolism and enrich the metabolic profile of cxurcumin in vivo,we carried out this research.A systematic method with highly sensitive UPLC-Q/TOF-MS was established to analyze different biological samples of rats after展开更多
A simple,rapid and sensitive liquid chromatography with tandem mass spectrometry method for the determination of periplocymarin in human blood and urine was developed.The digoxin‑d3 was used as an internal standard.Pe...A simple,rapid and sensitive liquid chromatography with tandem mass spectrometry method for the determination of periplocymarin in human blood and urine was developed.The digoxin‑d3 was used as an internal standard.Periplocymarin and digoxin‑d3(IS)were processed with ethyl acetate by liquid–liquid extraction.The chromatographic separation was performed on a Shim‑pack XR‑ODSIII C18 column with a 7 min gradient elution using methanol‑ammonium formate(5 mmol/L)as mobile phase at a flow rate of 0.3 mL/min(65:35,v/v).The detection was performed on a triple quadrupole tandem mass spectrometer using positive‑ion mode electrospray ionization in selected reaction monitoring mode.The periplocymarin was well separated from the internal standard.Two calibration curves were linear within the concentration range 0.01–1µg/mL.The limit of detection and quantification of blood and urine samples were both estimated at 0.005 and 0.01µg/mL.The interday and intraday precisions,accuracy,and recovery were assessed to verify this method.The results showed that the method was suitable for the determination of periplocymarin in forensic toxicological analysis and clinical diagnosis.展开更多
AIM: To identify differentially expressed hydrophobic proteins in colorectal cancer. METHODS: Eighteen pairs of colorectal cancerous tissues in addition to tissues from normal mucosa were analysed. Hydrophobic protein...AIM: To identify differentially expressed hydrophobic proteins in colorectal cancer. METHODS: Eighteen pairs of colorectal cancerous tissues in addition to tissues from normal mucosa were analysed. Hydrophobic proteins were extracted from the tissues, separated using 2-D gel electrophoresis and analysed using Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS). Statistical analysis of the proteins was carried out in order to determine the significance of each protein to colorectal cancer (CRC) and also their relation to CRC stages, grades and patients’ gender. RESULTS: Thirteen differentially expressed proteins which were expressed abundantly in either cancerous or normal tissues were identified. A number of these proteins were found to relate strongly with a particular stage or grade of CRC. In addition, the association of these proteins with patient gender also appeared to be significant.CONCLUSION: Stomatin-like protein 2 was found to be a promising biomarker for CRC, especially in female patients. The differentially expressed proteins identified were associated with CRC and may act as drug target candidates.展开更多
Huperzine A is a potent, reversible, and blood-brain barrier permeable acetylcholinesterase inhibitor. The aim of this study was to compare the pharmacokinetics, tolerability, and bioavailability of two formulations w...Huperzine A is a potent, reversible, and blood-brain barrier permeable acetylcholinesterase inhibitor. The aim of this study was to compare the pharmacokinetics, tolerability, and bioavailability of two formulations with the established reference formulation of huperzine A in a fasting, healthy Chinese male population. This was a randomized, single-dose, 3-period, 6-sequence crossover study. The plasma concentrations of huperzine A were determined by liquid chromatography tandem mass spectrometry. Tolerability was assessed based on subject interview, vital sign monitoring, physical examination, and routine blood and urine tests. The mean(SD) pharmacokinetic parameters of the reference drug were Cmax, 1.550(0.528) ng/m L; t1/2, 12.092(1.898) h; AUC0-72 h, 17.550(3.794) ng·h/m L. Those of the test formulation A and test formulation B were Cmax, 1.412(0.467), 1.521(0.608) ng/m L; t1/2, 12.073(2.068), 12.271(1.678) h; AUC0-72 h, 15.286(3.434) ng·h/mL, 15.673(3.586) ng·h/m L. The 90% confidence intervals for the AUC0-72 h and Cmax were between 0.80 and 1.25. No adverse events were reported by the subjects or found with results of clinical laboratory test. The test and reference products met the regulatory criteria for bioequivalence in these fasting, healthy Chinese male volunteers. All three formulations appeared to be well tolerated.展开更多
Endogenous ribonucleotides(RNs)and deoxyribonucleotides(dRNs)are important metabolites related to the pathogenesis of many diseases.In light of their physiological and pathological significances,a novel and sensitive ...Endogenous ribonucleotides(RNs)and deoxyribonucleotides(dRNs)are important metabolites related to the pathogenesis of many diseases.In light of their physiological and pathological significances,a novel and sensitive pre-column derivatization method with N-(t-butyldimethylsilyl)-N-methyltrifluoroacetamide(MTBSTFA)was developed to determine RNs and dRNs in human cells using high-performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS).A one-step extraction of cells with 85%methanol followed by a simple derivatization reaction within 5 min at room temperature contributed to shortened analysis time.The derivatives of 22 nucleoside mono-,di-and tri-phosphates were retained on the typical C;column and eluted by ammonium acetate and acetonitrile in 9 min.Under these optimal conditions,good linearity was achieved in the tested calibration ranges.The lower limit of quantitation(LLOQ)was determined to be 0.1-0.4μM for the tested RNs and 0.001-0.1μM for dRNs.In addition,the precision(CV)was<15%and the RSD of stability was lower than 10.4%.Furthermore,this method was applied to quantify the endogenous nucleotides in human colorectal carcinoma cell lines HCT 116 exposed to 10-hydroxycamptothecin.In conclusion,our method has proven to be simple,rapid,sensitive,and reliable.It may be used for specific expanded studies on intracellular pharmacology in vitro.展开更多
Clopidogrel is a pro-drug which needs two-step metabolism to produce the active thiol metabolite.This study aimed to explore an efficient method to simultaneously determine the plasma clopidogrel,2-oxo-clopidogrel(2-O...Clopidogrel is a pro-drug which needs two-step metabolism to produce the active thiol metabolite.This study aimed to explore an efficient method to simultaneously determine the plasma clopidogrel,2-oxo-clopidogrel(2-Oxo-CLP),and the clopidogrel active metabolite(CAM).A high-throughput liquid chromatography tandem mass spectrometry(LC-MS/MS)was therefore developed.The analytes were extracted from plasma by using methyl tert-butyl ether(MTBE).Chromatographic separation was performed on a C18 column under an isocratic elution,accompanied with acetonitrile and deionized water containing 0.1%formic acid.After optimizing the condition of LC-MS/MS,a stable linearity was observed in the standard curves over the concentration ranges of 0.05 to 50.0 ng/mL for clopidogrel,0.5 to 50.0 ng/mL for 2-Oxo-CLP,and 0.5 to 100 ng/mL for clopidogrel active metabolite derivative(CAMD).The retention time was 4.78 minutes,3.79 minutes,3.59 minutes,and 4.82 minutes for clopidogrel,2-Oxo-CLP,CAMD,and internal standard,respectively.Both the relative standard deviation and the relative error were within the requirement of operating criteria.No significant degradation of clopidogrel,2-Oxo-CLP,and CAMD occurred under different storage conditions.This method was successfully validated in 3 patients with coronary artery disease.The results showed that the current LC-MS/MS method was efficient for simultaneously detecting clopidogrel,2-Oxo-CLP,and CAM with fine linearity,accuracy,precision,and stability.展开更多
As lipidomics has attracted increased attention in life science,advanced mass spectrometry(MS)technologies have been combined with other separation techniques to improve and expand the branch of study.This review inte...As lipidomics has attracted increased attention in life science,advanced mass spectrometry(MS)technologies have been combined with other separation techniques to improve and expand the branch of study.This review intends to provide general knowledge of offline and online coupling of flow field-flow fractionation(FlFFF)—a technique that encompasses the separation of nano-to micro-scale biomolecules—with MS for analysis of blood plasma lipoproteins,processes that are considered bottomup and top-down approaches,respectively.The first part of this review focuses on the bottom-up method using multiplexed hollow fiber FlFFF(MxHF5)and nanoflow liquid chromatography electrospray-ionization tandem mass spectrometry(nLC-ESI–MS/MS)for non-targeted identification of lipids.In this protocol,plasma lipoproteins of different types are collected using MxHF5,and the lipids within the lipoproteins are then extracted and analyzed via nLC-ESI–MS/MS.The second part of the review describes the top-down approach,which uses online coupling of miniaturized FlFFF to ESI–MS for a fast screening of targeted lipids.Here,the separation of lipoproteins and detection of their component lipids are achieved simultaneously.While both methods aim to quantify the lipids within lipoproteins,the bottom-up approach provides an extensive lipidome,whereas the top-down method is suitable for high-speed targeted lipidomic analysis.This review discusses variants of FlFFF-ESI–MS/MS that offer effective analytical technologies for lipidomics.展开更多
A highly sensitive and selective high performance liquid chromatography–tandem mass spectrometry method was developed and validated for the quantification of alverine(ALV) and its active metabolite, para hydroxy al...A highly sensitive and selective high performance liquid chromatography–tandem mass spectrometry method was developed and validated for the quantification of alverine(ALV) and its active metabolite, para hydroxy alverine(PHA), in human plasma. For sample preparation, solid phase extraction of analytes was performed on Phenomenex Strata-X cartridges using alverine-d5 as the internal standard. The analytes were separated on Symmetry Shield RP18(150 mm×3.9 mm, 5 μm) column with a mobile phase consisting of acetonitrile and10 mM ammonium formate(65:35, v/v). Detection and quantitation was done by electrospray ionization mass spectrometry in the positive mode using multiple reaction monitoring. The assay method was fully validated over the concentration range of 15.0–15,000 pg/mL for ALV and 30.0–15,000 pg/mL for PHA. The intra-day and inter-day accuracy and precision(% CV) ranged from 94.00% to 96.00% and 0.48% to 4.15% for both the analytes. The mean recovery obtained for ALV and PHA was 80.59% and 81.26%, respectively. Matrix effect,expressed as IS-normalized matrix factor ranged from 0.982 to 1.009 for both the analytes. The application of the method was demonstrated for the specific analysis of ALV and PHA for a bioequivalence study in 52 healthy subjects using 120 mg ALV capsules. The assay reproducibility was also verified by reanalysis of 175 incurred subject samples.展开更多
L-Ergothioneine(L-EGT)possesses excellent antioxidant activity and has been used in the food,pharmaceuticals and cosmetics industries.In this study,a new efficient and sensitive ultra-performance liquid chromatography...L-Ergothioneine(L-EGT)possesses excellent antioxidant activity and has been used in the food,pharmaceuticals and cosmetics industries.In this study,a new efficient and sensitive ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method was established for the quantitative determination of L-EGT in food.The sample was extracted with methanol-water(70:30,V/V),separated by hydrophilic interaction liquid chromatography(HILIC)and detected by triple-quadrupole mass spectrometry.Validation studies were carried out on different product and the limit of quantitation was 20μg/kg(milk,alcohol-free beverages,dairy products)and 40µg/kg(cereal bars,chocolate).Excellent linearity(correlation coefficient(R2)≥0.999)was achieved for L-EGT quantification in the range of 5–200 ng/mL.The recoveries of the method(83.7%−107.5%)and the relative standard deviation(RSD,0.88%−6.84%(n=6))meet the performance criteria required for the determination of L-EGT in food.Finally,the applicability of the method was tested by analysing actual samples.In general,the method developed is simple,reliable,accurate,and stable and could be useful for routine analyses of L-EGT in food.展开更多
Jatropha curcas is an important economic plant for biodiesel, which is extracted mainly from the endosperm of its mature seeds. Despite the morphological and functional differences between the embryo and endosperm, pr...Jatropha curcas is an important economic plant for biodiesel, which is extracted mainly from the endosperm of its mature seeds. Despite the morphological and functional differences between the embryo and endosperm, proteomic characteristics of the two tissues are not yet known. Similar proteomic profiles were observed in the two-dimensional gel electrophoresis maps from the two tissues. There were 380 and 533 major protein spots in the embryo and endosperm, respectively. Fourteen identical spots, showing a notable change, were selected and identified by tandem mass spectrometry. Among these proteins, dihydrolipoamide acetyltransferase (spot 27) participates in tricarboxylic acid cycle, which is an amphibolic pathway. The two parts both included proteins related to stress (spots 8, 115, 118, 125, 130) and signal transduction (spots 7, 100, 108). According to the volume percentage of proteins in embryo and endosperm, the proteins in endosperm (spots 54, 61, 73) were catabolism-related enzymes and reserves to provide the nutrition for seed germination; the proteins in embryo (spots 27, 62, 122) were inclined to anabolism and utilized the nutrition from the endosperm to generate a new life.展开更多
Perfluorinated compounds(PFCs)are ubiquitously distributed in the environment mainly as perfluorocarboxylic acids(PFCAs)and perfluoroalkyl sulfonates(PFASs).In this paper,six PFCAs and two PFASs were quantified in sur...Perfluorinated compounds(PFCs)are ubiquitously distributed in the environment mainly as perfluorocarboxylic acids(PFCAs)and perfluoroalkyl sulfonates(PFASs).In this paper,six PFCAs and two PFASs were quantified in surface and tap water samples from 12 sites around Lake Taihu near Shanghai City in East China.Predominant PFCs were perfluorooctanoic acid(PFOA)and perfluorooctane sulfonate(PFOS),of which the concentration ranges were 6.8–206 and 1.2–45 ng·L^(–1),the geometric means were 35.3 and 9.4 ng·L^(–1),and the median(quartile range)values were 31.4(34.4)and 10.4(10.7)ng·L^(–1),respectively.Other PFCs were also detected but in much lower concentrations than PFOA.The sources of the PFCs were expected to be direct industrial discharges in the Lake Taihu area,and this area was also a possible source of PFCs contaminations in Shanghai district in the downstream.PFCs distributions were found different in the upstream,downstream and north part of Lake Taihu.Occurrences of PFCs in the tap water in Lake Taihu area indicated their exposure to the local people.A brief estimation of the environmental risks by PFCs implied no acute or immediate risks from PFCs to local human health,but chronic risks from PFOA in the tap water should be considered in the downstream regions.展开更多
Fenugreek, a traditional Chinese medical plant, has been widely used as food ingredients because of its out- standing medicinal qualities. The hypoglycemic activity of fenugreek is one of its important pharmacological...Fenugreek, a traditional Chinese medical plant, has been widely used as food ingredients because of its out- standing medicinal qualities. The hypoglycemic activity of fenugreek is one of its important pharmacological properties. Both of saponin and flavonoid components have the hypoglycemic activity and their contents in fenugreek are 4%--8% and 1% ---2%, respectively. This paper focused on these two types of components to carry out purification research and chemical analysis. The heating reflux extraction method and macroporous resin purification method were designed to prepare the saponins and the flavonoids components from defatted fenugreek seeds. Petroleum ether ultrasonic skim and 70% ethanol refluxing were used for the extraction of saponins and flavonoid from fenugreek. The column of DM130 macroporous resin and D101 macroporous resin were respectively used to prepare fenugreek saponin and flavonoid components, and the total contents of them were 78.56% and 62.28%, respectively. The saponin and flavonoids were subsequently analyzed by an ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS) along with an ultra-performance liquid chromatography and ion-trap tandem mass spectrometry(UPLC-IT-MS"). As a result, 57 saponins and 19 flavonoid compounds were characterized. The obtained results will provide a theory basis for further research on fenugreek, as well as research and development of hypogly- cemic new drugs.展开更多
基金Supported by the Projects of the General Administration of Quality Supervision,Inspection and Quarantine of China(No.2007IK157)
文摘Eighteen sex hormones in antler velvet were determined by high performance liquid chromatography tandem mass spectrometry.The solid phase extraction was applied to eliminating the matrix effect.The experimental conditions were examined and optimized.Under the optimal conditions,the proposed method provides the good linearities and determination limits(0.2―1.0 μg/kg) of the analytes investigated.The recoveries ranging from 72.3% to 149.5% were obtained for the target analytes at two concentration levels.This method was applied to the determination of eighteen sex hormones in different kinds of antler velvet samples and the obtained results are satisfactory.The results indicate that the proposed method is suitable for the determination of sex hormones in antler velvet samples.
基金the supports of the National Key Research and Development of BioBased Rubber(2017YFB0306900&2017YFB0306901)the National Natural Science Foundation of China(51673012)+1 种基金the Fundamental Research Funds for the Central Universities(PYBZ1828)the Beijing Technology and Business Universtiy Youth Scholoars Funds(PXM2019014213000007)。
文摘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.
文摘A reliable,selective and sensitive liquid chromatography tandem mass spectrometry method was developed and validated for the quantification of lamotrigine in human plasma using lamotrigine13C3,d3 as an internal standard.Analyte and internal standard were extracted from human plasma by solid-phase extraction and detected in positive ion mode by tandem mass spectrometry with electrospray ionization(ESI) interface.Chromatographic separation was performed on a Chromolith s SpeedROD;RP-18e column(50-4.6 mm i.d.) using acetonitrile:570.1 mM ammonium formate solution(90:10,v/v) as the mobile phase at a flow rate of 0.500 mL/min.The calibration curves were linear over the range of 5.02-1226.47 ng/mL with the lower limit of quantitation validated at 5.02 ng/mL.The analytes were found stable in human plasma through three freeze(-20℃)-thaw(ice-cold water bath) cycles and under storage on bench-top in ice-cold water bath for at least 6.8 h,and also in the mobile phase at 10℃ for at least 57h.The method has shown good reproducibility,as the intra-and inter-day precisions were within 3.0%,while the accuracies were within 76.0% of nominal values.The validated LC-MS/MS method was applied for the evaluation of pharmacokinetic and bioequivalence parameters of lamotrigine after an oral administration of 50mg lamotrigine tablet to thirty-two healthy adult male volunteers.
文摘A rapid and sensitive liquid chromatography tandem mass spectrometry(LC-MS/MS) method has been developed and validated for the determination of moxifloxacin(MOXI) in human plasma. After a simple protein precipitation using acetonitrile, the post treatment samples were analysed on a C18 column interfaced with a Triple Quadropole Tandem Mass Spectrometer. Positive electrospray ionization was employed as the ionization source. The mobile phase consisted of 0.1% formic acid–acetonitrile(60:40, v/v). Ciprofloxacin(CIPRO) was used as an internal standard. The analyte and internal standard(CIPRO) were monitored in the multiple reaction monitoring mode(MRM). The mass transition ion-pair has been followed as m/z 402→358.2 for MOXI and 332→288.1 for CIPRO. The method was linear in the concentration range of 25–5000 ng/mL. The lower limit of quantification was 25 ng/mL. The intra- and inter-day precision(relative standard deviation) and accuracy(relative error) values were within 12.4%. Each plasma sample was analyzed within 3 min.
基金supported financially by the National Natural Science Foundation of China (Grant No. 81973604, 81803690and 81703684)the Innovative Talents Funding of Heilongjiang University of Chinese Medicine(Grant No.2018RCD25)+8 种基金the National natural science foundation matching project (Grant No. 2018PT02)the National natural Science Foundation Matching Project (Grant No. 2017PT01)the Graduate Innovative Research Project Foundation of Heilongjiang University of Chinese Medicine (Grant No. 2019yjscx013)the Postdoctoral Initial Fund of Heilongjiang Provincethe University Nursing Program for Young Scholars with Creative Talents in Heilongjiang Province (Grant No. UNPYSCT2017215 and UNPYSCT2017219)the Natural Science Foundation of Heilongjiang Province (Grant No. H2015037)the Heilongjiang University of Chinese Medicine Doctoral Innovation Foundation (Grant No. 2014bs05)the Application Technology Research and Development Projects of Harbin Technology Bureau (Grant No. 2014RFQXJ149)Heilongjiang Postdoctoral Scientific Research Developmental Fund (Grant No.LBHQ16210 and LBH-Q17161)
文摘A rapid and high selective ultra-performance liquid chromatography(UPLC)with tandem mass spectrometry method for simultaneous determination of six compounds including albiflorin,paeoniflorin,picroside I,picroside II,saikosaponin A,and saikosaponin D in rat plasma was developed and validated using butyl p-hydroxybenzoate as an internal standard.One-step direct protein precipitation with acetonitrile was used to extract the compounds from the rat plasma samples.Chromatographic separation was achieved using an ACQUITY UPLC BEH C18 column(100 mm×2.1 mm,1.7μm)at a flow rate of 0.4 m L/min,using gradient mode containing 0.1%formic acid in water and acetonitrile were used as the Mobile phase A and B.Electrospray ionization in negative ion mode and multiple reaction monitoring were used to identify and quantify active components.Calibration curves showed good linearity(R^2>0.9908)over a wide concentration range for all compounds.The intra-and interday precision(relative standard deviation)ranged 2.4%–7.0%and 2.6%–8.0%,respectively.The accuracy(relative error)was from-13.0%to 13.2%at all quality control levels.The recovery ranged from 81.1%to 92.5%.The validated method was successfully applied to pharmacokinetic study in rats after oral administration of Qing Gan-Shu Yu-Fang.The results show that one can draw a conclusion that these six active ingredients can be quickly absorbed and play a pharmacodynamic role rapidly in vivo.
基金supported by the National Nature Science Foundation of China (No.21075074)
文摘Aspartame is a widely used sweetener, the long-term safety of which has been controversial ever since it was accepted for human consumption. It is unstable and can produce some harmful degradation products under certain storage conditions. A high-performance liquid chromatography/tandem mass spectrometry method was developed for the simultaneous analysis of aspartame and its four degradation products, including aspartic acid, phenylalanine, aspartyl-phenylalanine and 5-benzyl-3,6- dioxo-2-piperazieacetic acid in water and in diet soft drinks. Aspartame and its four degradation products were quantified by a matrix matched external standard calibration curve with excellent correlation coefficients. The limits of detection were 0.16-5.8 μg/L, which exhibited higher sensitivity than common methods. This method was rapid, sensitive, specific and capable of eliminating matrix interferences. It was also applied to the study of the degradation of aspartame at various pH and temperatures. The results indicated that aspartame was partly degraded under strong acidic or basic conditions and the extent of degradation increased with increasing temperature.
基金Supported by the National Key Research and Development Program of China(No.2016YFF0201104)the Construction of Public Service Platform for Research and Test of Marine Pilot Technology of China(No.Bhsfs009)the Project of Xiamen Southern oceanographic Center,China(No.16PFW008SF15).
文摘A sensitive analytical method was developed to determine tetrodotoxin(TTX) in human plasma samples using protein precipitation, followed by ultra performance liquid chromatography(UPLC) analysis coupled with tandem mass spectrometry(MS/MS) using 11-deoxytetrodotoxin(11-deoxyTTX) as an internal standard. The plasma samples were prepared using protein precipitation prior to being analyzed by UPLC-MSfMS to identify TTX over a zwitterionic-hydrophilic interaction liquid chromatography column. The retention time values of TTX and 11-deoxyTTX were 4.12 and 3.67 min, respectively. TTX and 11-deoxyTTX were monitored and quantitated on the basis of their ion transitions for their respective precursor ions to their product ions(i.e., m/z 320.0→162. l for TTX and m/z 304.0→176.0 for 11-deoxyTTX) in the multiple reaction-monitoring mode. The lower limit of quantification of this method was determined to be 0.0199 ug/mL. This method showed good linearity for plasma samples that contained TTX concentrations in the range of 0.0199--1.99 ng/mL. The specificity, precision, accuracy, matrix effect, and stability characteristics of this method were also examined. The intra-assay precision and accuracy ranged from 1.89% to 6.00% and from 92.21% to 100.00%, whereas the inter-assay precision and accuracy ranged from 0.64% to 7.75% and from 99.38% to 101.26%, respectively. This new method therefore represents a rapid, accurate, reliable, and highly sensitive method for the qualitative and quantitative analyses of a trace amount of TTX in human plasma samples.
基金partly supported by National Natural Science Foundation of China(No.81430095)also by Special National Program on Key Basic Research Project(No.2014CB560706)
文摘Curcumin,a safe natural yellow pigment with a wide range of pharmacological activities,is used both in herbal drugs and as a food coloring agents.Studies have shown that curcumin would suffer from extensive metabolism in vivoand the predominant metabolic pathways are reduction and conjugation.In order to comprehensively study the metabolism and enrich the metabolic profile of cxurcumin in vivo,we carried out this research.A systematic method with highly sensitive UPLC-Q/TOF-MS was established to analyze different biological samples of rats after
基金supported by the Project of the National Natural Sciences Foundation of China(81373239).
文摘A simple,rapid and sensitive liquid chromatography with tandem mass spectrometry method for the determination of periplocymarin in human blood and urine was developed.The digoxin‑d3 was used as an internal standard.Periplocymarin and digoxin‑d3(IS)were processed with ethyl acetate by liquid–liquid extraction.The chromatographic separation was performed on a Shim‑pack XR‑ODSIII C18 column with a 7 min gradient elution using methanol‑ammonium formate(5 mmol/L)as mobile phase at a flow rate of 0.3 mL/min(65:35,v/v).The detection was performed on a triple quadrupole tandem mass spectrometer using positive‑ion mode electrospray ionization in selected reaction monitoring mode.The periplocymarin was well separated from the internal standard.Two calibration curves were linear within the concentration range 0.01–1µg/mL.The limit of detection and quantification of blood and urine samples were both estimated at 0.005 and 0.01µg/mL.The interday and intraday precisions,accuracy,and recovery were assessed to verify this method.The results showed that the method was suitable for the determination of periplocymarin in forensic toxicological analysis and clinical diagnosis.
基金Supported by RU Grant, No.1001/PFARMASI/815007 and Universiti Sains Malaysia
文摘AIM: To identify differentially expressed hydrophobic proteins in colorectal cancer. METHODS: Eighteen pairs of colorectal cancerous tissues in addition to tissues from normal mucosa were analysed. Hydrophobic proteins were extracted from the tissues, separated using 2-D gel electrophoresis and analysed using Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS). Statistical analysis of the proteins was carried out in order to determine the significance of each protein to colorectal cancer (CRC) and also their relation to CRC stages, grades and patients’ gender. RESULTS: Thirteen differentially expressed proteins which were expressed abundantly in either cancerous or normal tissues were identified. A number of these proteins were found to relate strongly with a particular stage or grade of CRC. In addition, the association of these proteins with patient gender also appeared to be significant.CONCLUSION: Stomatin-like protein 2 was found to be a promising biomarker for CRC, especially in female patients. The differentially expressed proteins identified were associated with CRC and may act as drug target candidates.
文摘Huperzine A is a potent, reversible, and blood-brain barrier permeable acetylcholinesterase inhibitor. The aim of this study was to compare the pharmacokinetics, tolerability, and bioavailability of two formulations with the established reference formulation of huperzine A in a fasting, healthy Chinese male population. This was a randomized, single-dose, 3-period, 6-sequence crossover study. The plasma concentrations of huperzine A were determined by liquid chromatography tandem mass spectrometry. Tolerability was assessed based on subject interview, vital sign monitoring, physical examination, and routine blood and urine tests. The mean(SD) pharmacokinetic parameters of the reference drug were Cmax, 1.550(0.528) ng/m L; t1/2, 12.092(1.898) h; AUC0-72 h, 17.550(3.794) ng·h/m L. Those of the test formulation A and test formulation B were Cmax, 1.412(0.467), 1.521(0.608) ng/m L; t1/2, 12.073(2.068), 12.271(1.678) h; AUC0-72 h, 15.286(3.434) ng·h/mL, 15.673(3.586) ng·h/m L. The 90% confidence intervals for the AUC0-72 h and Cmax were between 0.80 and 1.25. No adverse events were reported by the subjects or found with results of clinical laboratory test. The test and reference products met the regulatory criteria for bioequivalence in these fasting, healthy Chinese male volunteers. All three formulations appeared to be well tolerated.
基金supported by Science and Technology Development Fund, Macao SAR (File Nos.: 0052/2018/A2 and 0077/2019/ A2)the National Natural Science Foundation of China (Grant No.: 61827819)
文摘Endogenous ribonucleotides(RNs)and deoxyribonucleotides(dRNs)are important metabolites related to the pathogenesis of many diseases.In light of their physiological and pathological significances,a novel and sensitive pre-column derivatization method with N-(t-butyldimethylsilyl)-N-methyltrifluoroacetamide(MTBSTFA)was developed to determine RNs and dRNs in human cells using high-performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS).A one-step extraction of cells with 85%methanol followed by a simple derivatization reaction within 5 min at room temperature contributed to shortened analysis time.The derivatives of 22 nucleoside mono-,di-and tri-phosphates were retained on the typical C;column and eluted by ammonium acetate and acetonitrile in 9 min.Under these optimal conditions,good linearity was achieved in the tested calibration ranges.The lower limit of quantitation(LLOQ)was determined to be 0.1-0.4μM for the tested RNs and 0.001-0.1μM for dRNs.In addition,the precision(CV)was<15%and the RSD of stability was lower than 10.4%.Furthermore,this method was applied to quantify the endogenous nucleotides in human colorectal carcinoma cell lines HCT 116 exposed to 10-hydroxycamptothecin.In conclusion,our method has proven to be simple,rapid,sensitive,and reliable.It may be used for specific expanded studies on intracellular pharmacology in vitro.
基金This work was supported by National Natural Science Funding of China(Grant No.81170181)the Jiangsu Province's Key Provincial Talents Program(Grant No.ZDRCA2016013)+2 种基金the Second Level of 333 High Level Talent Training Project in Jiangsu Province(Grant No.BRA2019099)Special Fund for Key R&D Plans(Social Development)of Jiangsu Province(Grant No.BE2019754)a Project Funded by the Priority Academic Program Development of Jiangsu Higher Education Institutes.
文摘Clopidogrel is a pro-drug which needs two-step metabolism to produce the active thiol metabolite.This study aimed to explore an efficient method to simultaneously determine the plasma clopidogrel,2-oxo-clopidogrel(2-Oxo-CLP),and the clopidogrel active metabolite(CAM).A high-throughput liquid chromatography tandem mass spectrometry(LC-MS/MS)was therefore developed.The analytes were extracted from plasma by using methyl tert-butyl ether(MTBE).Chromatographic separation was performed on a C18 column under an isocratic elution,accompanied with acetonitrile and deionized water containing 0.1%formic acid.After optimizing the condition of LC-MS/MS,a stable linearity was observed in the standard curves over the concentration ranges of 0.05 to 50.0 ng/mL for clopidogrel,0.5 to 50.0 ng/mL for 2-Oxo-CLP,and 0.5 to 100 ng/mL for clopidogrel active metabolite derivative(CAMD).The retention time was 4.78 minutes,3.79 minutes,3.59 minutes,and 4.82 minutes for clopidogrel,2-Oxo-CLP,CAMD,and internal standard,respectively.Both the relative standard deviation and the relative error were within the requirement of operating criteria.No significant degradation of clopidogrel,2-Oxo-CLP,and CAMD occurred under different storage conditions.This method was successfully validated in 3 patients with coronary artery disease.The results showed that the current LC-MS/MS method was efficient for simultaneously detecting clopidogrel,2-Oxo-CLP,and CAM with fine linearity,accuracy,precision,and stability.
基金Grant from the National Research Foundation of Korea(NRF-2015R1A2A1A01004677).
文摘As lipidomics has attracted increased attention in life science,advanced mass spectrometry(MS)technologies have been combined with other separation techniques to improve and expand the branch of study.This review intends to provide general knowledge of offline and online coupling of flow field-flow fractionation(FlFFF)—a technique that encompasses the separation of nano-to micro-scale biomolecules—with MS for analysis of blood plasma lipoproteins,processes that are considered bottomup and top-down approaches,respectively.The first part of this review focuses on the bottom-up method using multiplexed hollow fiber FlFFF(MxHF5)and nanoflow liquid chromatography electrospray-ionization tandem mass spectrometry(nLC-ESI–MS/MS)for non-targeted identification of lipids.In this protocol,plasma lipoproteins of different types are collected using MxHF5,and the lipids within the lipoproteins are then extracted and analyzed via nLC-ESI–MS/MS.The second part of the review describes the top-down approach,which uses online coupling of miniaturized FlFFF to ESI–MS for a fast screening of targeted lipids.Here,the separation of lipoproteins and detection of their component lipids are achieved simultaneously.While both methods aim to quantify the lipids within lipoproteins,the bottom-up approach provides an extensive lipidome,whereas the top-down method is suitable for high-speed targeted lipidomic analysis.This review discusses variants of FlFFF-ESI–MS/MS that offer effective analytical technologies for lipidomics.
基金the support and necessary facilities provided by Accutest Research Lab,Ahmedabad
文摘A highly sensitive and selective high performance liquid chromatography–tandem mass spectrometry method was developed and validated for the quantification of alverine(ALV) and its active metabolite, para hydroxy alverine(PHA), in human plasma. For sample preparation, solid phase extraction of analytes was performed on Phenomenex Strata-X cartridges using alverine-d5 as the internal standard. The analytes were separated on Symmetry Shield RP18(150 mm×3.9 mm, 5 μm) column with a mobile phase consisting of acetonitrile and10 mM ammonium formate(65:35, v/v). Detection and quantitation was done by electrospray ionization mass spectrometry in the positive mode using multiple reaction monitoring. The assay method was fully validated over the concentration range of 15.0–15,000 pg/mL for ALV and 30.0–15,000 pg/mL for PHA. The intra-day and inter-day accuracy and precision(% CV) ranged from 94.00% to 96.00% and 0.48% to 4.15% for both the analytes. The mean recovery obtained for ALV and PHA was 80.59% and 81.26%, respectively. Matrix effect,expressed as IS-normalized matrix factor ranged from 0.982 to 1.009 for both the analytes. The application of the method was demonstrated for the specific analysis of ALV and PHA for a bioequivalence study in 52 healthy subjects using 120 mg ALV capsules. The assay reproducibility was also verified by reanalysis of 175 incurred subject samples.
基金This work was supported by National Key Research and Development Program of China(2019YFC1606400).
文摘L-Ergothioneine(L-EGT)possesses excellent antioxidant activity and has been used in the food,pharmaceuticals and cosmetics industries.In this study,a new efficient and sensitive ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method was established for the quantitative determination of L-EGT in food.The sample was extracted with methanol-water(70:30,V/V),separated by hydrophilic interaction liquid chromatography(HILIC)and detected by triple-quadrupole mass spectrometry.Validation studies were carried out on different product and the limit of quantitation was 20μg/kg(milk,alcohol-free beverages,dairy products)and 40µg/kg(cereal bars,chocolate).Excellent linearity(correlation coefficient(R2)≥0.999)was achieved for L-EGT quantification in the range of 5–200 ng/mL.The recoveries of the method(83.7%−107.5%)and the relative standard deviation(RSD,0.88%−6.84%(n=6))meet the performance criteria required for the determination of L-EGT in food.Finally,the applicability of the method was tested by analysing actual samples.In general,the method developed is simple,reliable,accurate,and stable and could be useful for routine analyses of L-EGT in food.
基金Supported by the National Natural Science Foundation of China (U0733005)the Knowledge Innovation Program of the Chinese Academy of Sciences(KSCX2-YW-G-027, KSCX2-YW-G-035)
文摘Jatropha curcas is an important economic plant for biodiesel, which is extracted mainly from the endosperm of its mature seeds. Despite the morphological and functional differences between the embryo and endosperm, proteomic characteristics of the two tissues are not yet known. Similar proteomic profiles were observed in the two-dimensional gel electrophoresis maps from the two tissues. There were 380 and 533 major protein spots in the embryo and endosperm, respectively. Fourteen identical spots, showing a notable change, were selected and identified by tandem mass spectrometry. Among these proteins, dihydrolipoamide acetyltransferase (spot 27) participates in tricarboxylic acid cycle, which is an amphibolic pathway. The two parts both included proteins related to stress (spots 8, 115, 118, 125, 130) and signal transduction (spots 7, 100, 108). According to the volume percentage of proteins in embryo and endosperm, the proteins in endosperm (spots 54, 61, 73) were catabolism-related enzymes and reserves to provide the nutrition for seed germination; the proteins in embryo (spots 27, 62, 122) were inclined to anabolism and utilized the nutrition from the endosperm to generate a new life.
基金the National Science and Technology Pillar Program of China(Grant No.2006BAC19B06)the Major Projects on Control and Rectification of Water Body Pollution(2009ZX07313-003).
文摘Perfluorinated compounds(PFCs)are ubiquitously distributed in the environment mainly as perfluorocarboxylic acids(PFCAs)and perfluoroalkyl sulfonates(PFASs).In this paper,six PFCAs and two PFASs were quantified in surface and tap water samples from 12 sites around Lake Taihu near Shanghai City in East China.Predominant PFCs were perfluorooctanoic acid(PFOA)and perfluorooctane sulfonate(PFOS),of which the concentration ranges were 6.8–206 and 1.2–45 ng·L^(–1),the geometric means were 35.3 and 9.4 ng·L^(–1),and the median(quartile range)values were 31.4(34.4)and 10.4(10.7)ng·L^(–1),respectively.Other PFCs were also detected but in much lower concentrations than PFOA.The sources of the PFCs were expected to be direct industrial discharges in the Lake Taihu area,and this area was also a possible source of PFCs contaminations in Shanghai district in the downstream.PFCs distributions were found different in the upstream,downstream and north part of Lake Taihu.Occurrences of PFCs in the tap water in Lake Taihu area indicated their exposure to the local people.A brief estimation of the environmental risks by PFCs implied no acute or immediate risks from PFCs to local human health,but chronic risks from PFOA in the tap water should be considered in the downstream regions.
文摘Fenugreek, a traditional Chinese medical plant, has been widely used as food ingredients because of its out- standing medicinal qualities. The hypoglycemic activity of fenugreek is one of its important pharmacological properties. Both of saponin and flavonoid components have the hypoglycemic activity and their contents in fenugreek are 4%--8% and 1% ---2%, respectively. This paper focused on these two types of components to carry out purification research and chemical analysis. The heating reflux extraction method and macroporous resin purification method were designed to prepare the saponins and the flavonoids components from defatted fenugreek seeds. Petroleum ether ultrasonic skim and 70% ethanol refluxing were used for the extraction of saponins and flavonoid from fenugreek. The column of DM130 macroporous resin and D101 macroporous resin were respectively used to prepare fenugreek saponin and flavonoid components, and the total contents of them were 78.56% and 62.28%, respectively. The saponin and flavonoids were subsequently analyzed by an ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS) along with an ultra-performance liquid chromatography and ion-trap tandem mass spectrometry(UPLC-IT-MS"). As a result, 57 saponins and 19 flavonoid compounds were characterized. The obtained results will provide a theory basis for further research on fenugreek, as well as research and development of hypogly- cemic new drugs.