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An ultra-robust fingerprinting method for quality assessment of traditional Chinese medicine using multiple reaction monitoring mass spectrometry

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Journal of Pharmaceutical Analysis 2021年第1期11卷 88-95页

作者： Zhenhao Li Xiaohui Zhang Jie Liao Xiaohui Fan Yiyu Cheng Pharmaceutical Informatics Institute College of Pharmaceutical SciencesZhejiang UniversityHangzhou310058China

Chromatographic fingerprinting has been perceived as an essential tool for assessing quality and chemical equivalence of traditional Chinese ***,this pattern-oriented approach still has some weak points in terms of chemical coverage and *** this work,we proposed a multiple reaction monitoring(MRM)-based fingerprinting method in which approximately 100 constituents were simultaneously detected for quality *** derivative MRM approach was employed to rapidly design MRM transitions independent of chemical standards,based on which the large-scale fingerprinting method was efficiently *** approach was exemplified on QiShenYiQi Pill(QSYQ),a traditional Chinese medicine-derived drug product,and its robustness was systematically evaluated by four indices:clustering analysis by principal component analysis,similarity analysis by the congruence coefficient,the number of separated peaks,and the peak area proportion of separated *** with conventional ultraviolet-based fingerprints,the MRM fingerprints provided not only better discriminatory capacity for the tested normal/abnormal QSYQ samples,but also higher robustness under different chromatographic conditions(i.e.,flow rate,apparent pH,column temperature,and column).The result also showed for such large-scale fingerprints including a large number of peaks,the angle cosine measure after min-max normalization was more suitable for setting a decision criterion than the unnormalized *** proof-of-concept application gives evidence that combining MRM technique with proper similarity analysis metrices can provide a highly sensitive,robust and comprehensive analytical approach for quality assessment of traditional Chinese medicine.

关键词： multiple reaction monitoring Mass spectrometry-based fingerprinting Quality assessment Traditional Chinese medicine Robustness evaluation

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Multiresidue pesticide analysis in tomato using GC-MS/MS using modified QuEChERS method with titanium-coated graphite with CNT-ABS nanocomposite as dispersive solid-phase extraction materials

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Food Quality and Safety 2022年第4期6卷 608-618页

作者： Mahadev C.Khetagoudar G.T.Deepa P.T.Goroji Mahadev B.Chetti Avvaru Praveen Kumar Dinesh C.Bilehal University of Agricultural Sciences DharwadKarnatakaIndia Department of Applied Chemistry School of Applied Natural ScienceAdama Science and Technology UniversityAdamaEthiopia Department of Chemistry Karnatak UniversityDharwadKarnatakaIndia

The presence of pesticide residues in food and vegetables is a growing concern for *** monitor these residues reliably,a selective and sensitive multiresidue system has been developed and validated in tomato by gas chromatography–tandem mass spectrometry(GC-MS/MS).Titanium-coated graphite with carbon nanotube(CNT)in acrylonitrile–butadiene–styrene(ABS)used as reversed-dispersive solid-phase extraction materials with modified QuEChERS(Quick,Easy,Cheap,Effective,Rugged,and Safe)***-coated graphite with CNT-ABS is synthesized,characterized by X-ray diffraction and scanning electron *** clean-up performance of titanium-coated graphite with CNT-ABS was demonstrated to be better to primary secondary amine and graphitized carbon black *** processing of two multiple reaction monitoring transformations for each analyte is done using GC-MS/MS in electron impact *** purification and recovery effects(74%–100%)of 35 pesticides were achieved in tomato matrices when using 5 mg of titanium-coated graphite ABS-CNT *** was observed that quinolphos and deltamethrin are present above the maximum residue *** technique proved to be reliable and sensitive in tomato samples for the routine testing of 35 pesticides.

关键词： Gas chromatography-tandem mass spectrometry pesticide residue analysis multiple reaction monitoring QuEChERS titanium-coated graphite with CNT-ABS nanocomposite

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Atmospheric pressure gas chromatography-tandem mass spectrometry analysis of fourteen emerging polycyclic aromatic sulfur heterocycles in PM_(2.5)

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Chinese Chemical Letters 2021年第2期32卷 801-804页

作者： Yanhao Zhang Yi-Jie Chen Yuanyuan Song Chuan Dong Zongwei Cai State Key Laboratory of Environmental and Biological Analysis Department of ChemistryHong Kong Baptist UniversityHong Kong SARChina Guangzhou Key Laboratory of Environmental Catalysis and Pollution Control School of Environmental Science and EngineeringInstitute of Environmental Health and Pollution ControlGuangdong University of TechnologyGuangzhou 510006China Institute of Environmental Science Shanxi UniversityTaiyuan 030006China

Research on pollution characteristics and toxicities of emerging polycyclic aromatic sulfur heterocycles(PASHs) in PM_(2.5) has not been reported due to the lack of analytical method with the needed *** the present study,a novel method for the determination of 14 PASHs in PM_(2.5) was developed using atmospheric pressure gas chro matography-tandem mass spectrometry(APGC-MS/MS).Atmospheric pressure chemical ionization was operated with multiple reaction monitoring in positive ionization *** sensitivity(method detection limit <1.673 pg/m^(3)),acceptable re coveries(67.6%-120.8%) and precisions(RSD of 2.2%-15.4%) were *** method was successfully applied for analyzing PASHs in 10 PM_(2.5) samples collected from Taiyuan,a typical industrial city in China,in 2016,The total concentrations were from 929 pg/m^(3) to 14,593 pg/m^(3).The determined levels indicated that further investigations on environmental fate and toxicities of PM_(2.5)-bound PASHs may be needed.

关键词： Atmospheric pressure gas chromatography-tandem mass spectrometry multiple reaction monitoring Polycyclic aromatic sulfur heterocycles PM_(2.5) Ambient concentrations

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Quantitative Evaluation of Aldo-keto Reductase Expression in Hepatocellular Carcinoma (HCC) Cell Lines

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Genomics, Proteomics & Bioinformatics 2013年第4期11卷 230-240页

作者： Lei Yang Ju Zhang Shenyan Zhang Weiwei Dong Xiaomin Lou Siqi Liu CAS Key Laboratory of Genome Sciences and Information Beijing Institute of Genomics Chinese Academy of Sciences Department of Oncology General Hospital of PLA

The involvement of aldo-keto reductases （AKRs） in tumorigenesis is widely reported, but their roles in the pathological process are not generally recognized due to inconsistent measure- ments of their expression. To overcome this problem, we simultaneously employed real-time PCR to examine gene expression and multiple reaction monitoring （MRM） of mass spectrometry （MS） to examine the protein expression of AKRs in five different hepatic cell lines. These include one rela- tively normal hepatic cell line, L-02, and four hepatocellular carcinoma （HCC） cell lines, HepG2, HUH7, BEL7402 and SMMC7721. The results of real-time PCR showed that expression of genes encoding the AKR1C family members rather than AKR1A and AKR1B was associated with tumor, and most of genes encoding AKRs were highly expressed in HUH7. Similar observations were obtained through MRM. Different from HUH7, the protein abundance of AKR1A and AKR1B was relatively consistent among the other four hepatic cell lines, while protein expression of AKR1C varied significantly compared to L-02. Therefore, we conclude that the abundant distri- bution of AKR 1C proteins is likely to be associated with liver tumorigenesis, and the AKR expres- sion status in HuH7 is completely different from other liver cancer cell lines. This study, for the first time, provided both overall and quantitative information regarding the expression of AKRs at both mRNA and protein levels in hepatic cell lines. Our observations put the previous use of AKRs as a biomarker into question since it is only consistent with our data from HUH7. Furthermore, the data presented herein demonstrated that quantitative evaluation and comparisons within a protein fam- ily at both mRNA and protein levels were feasible using current techniques.

关键词： Aldo-keto reductase HCC Quantitative analysis Real-time PCR multiple reaction monitoring

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Quantitative determination of multi-class bioactive constituents for quality control of Yiqi Jiangzhi Granules

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Chinese Herbal Medicines 2022年第2期14卷 324-331页

作者： Shaobo Guo Shaowei Hu Lijuan Jiang Xiaohe Chen Wei Zhang Yanyan Jiang Bin Liu School of Chinese Materia Medica Beijing University of Chinese MedicineBeijing 102488China

Objective:To establish a reliable and sensitive method for evaluating quality of Yiqi Jiangzhi Granules(YQJZG).Methods:Ultra performance liquid chromatography electrospray ionization tandem mass spectrometry(UPLC-ESI-MS/MS)was employed for simultaneous determination of eight marker *** was performed on an AQUITY UPLC;HSS T3 column,the mobile phase consisted of acetonitrile as the organic phase and 0.1%(volume percentage)formic acid as the *** marker components,ginsenoside Rg1(GRg1),ginsenoside Re(GRe),ginsenoside Rb1(Gb1),typhaneoside(TEO),isorhamnetin-3-O-neohespeidoside(IN),hesperidin(HPD),aurantio-obtusin-6-O-β-D-glucoside(AG)and curcumin(CCM),were detected by multiple reaction monitoring(MRM)*** Chinese Pharmacopoeia(2020 edition)was regarded as the guidance document for this method ***:The method showed good linearity(R^(2)≥0.9990).The relative standard deviation(RSD)values for the instrument precision,intermediate precision and repeatability were less than 2.91%,2.88%,and 3.54%,*** average recovery varied from 91.08%to 103.89%,with RSD below 3.81%.Sample solutions were found to be stable within 24 h at 4℃(RSD<2.85%).Eight marker components were successfully determined from three batches of ***:The proposed UPLC-ESI-MS/MS method was found to be simple,fast and sensitive,and can be used for the routine quality assessment of ***,this method may provide a new and powerful tool of quality control for other traditional Chinese medicine analogous formulae.

关键词： multiple reaction monitoring quality control traditional Chinese medicine UPLC-ESI-MS/MS Yiqi Jiangzhi Granules

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Identification and Determination of the Major Constituents in Xie-Bai-San by Ultra-performance Liquid Chromatography–Mass Spectrometry

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World Journal of Traditional Chinese Medicine 2024年第3期10卷 334-346页

作者： Bao-Xin Li Peng-Yue Li Li-Xia Hao Xiao-Xia Xue Sha-Sha Kong Qin-He Zhao Yun-Tao Dai Traditional Chinese Medicine Analysis Institute of Chinese Materia Medica China Academy of Chinese Medical Sciences

Objective: The ancient classical Chinese formulation, Xie-Bai-San(XBS), was studied qualitatively and quantitatively, and its main components were characterized. Materials and Methods: The chemical compounds in XBS were identified using a combination of ultra-performance liquid chromatography-quadrupole-Orbitrap mass spectrometry and molecular networking(MN) analysis. In addition, a multiple reaction monitoring(MRM) quantification method was established using ultra-high-performance liquid chromatography–triple quadrupole mass spectrometry. Mulberroside A, kukoamine B, liquiritin, and glycyrrhizic acid were quantitatively analyzed in ten batches of XBS using this method. Results: Using clusters of MN and databases, 91 compounds were rapidly identified, including stilbene glycosides, saponins,fiavonoids, and alkaloids. Of these, 30, 33, and 28 compounds were from Mori Cortex, Lycii Cortex, and Glycyrrhizae Radix et Rhizoma,respectively. The MRM scanning mode was used for the simultaneous sensitive quantitative determination of multiple components in a wide range of complex samples. The four main components were quantified using this method, which has good linearity. Conclusions: This study provides a comprehensive and reliable method for the identification and quantitative analysis of XBS.

关键词： Chemical constituent identification molecular networking multiple reaction monitoring quantitative analysis Xie-Bai-San

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Quantitative determination of four Sudan dyes in rat plasma with solid-phase extraction and UFLC-MS/MS analysis:Application to a pharmacokinetic study

Quantitative determination of four Sudan dyes in rat plasma ...

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中国毒理学会第六届全国毒理学大会

作者： ZHU Hao HUANG Kun-yu CHEN Xiao-hong ZHOU Lix-in JIN Mi-cong Medical School Ningbo University Zhejiang Provincial Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals Ningbo Key Laboratory of Poison Research and ControlNingbo Municipal Center for Disease Control and Prevention

OBJECTIVE To develop and validate for the simultaneous determination of four Sudan dyes(SudanⅠ,SudanⅡ,SudanⅢ,and SudanⅣ) in rat plasma for the first time,based on the ultra-fast liquid chromatography-tandem mass spectrometry(UFLC-MS/MS) method coupled with solid-phase extraction(SPE) procedure in order to reduce the complex matrix interferences and enrich the an-alytes. METHODS 30 rats were randomly assigned to five groups(blank edible oil group,SudanⅠgroup,SudanⅡgroup,SudanⅢgroup,and SudanlV group) with six rats(3 males and 3 females) *** dyes(SudanⅠ,SudanⅡ,SudanⅢ,and SudanlV) were separately dissolved in 10 mg·ml edible oil and administered via a single oral(po) dose of 50.0 mg·kg to Sprague-Dawley(SD) *** 20.0μl of the rat blood sample(at 10.0,20.0,30.0,and 40.0 min and 1.0,1.5, 2.0,3.0,5.0,7.0,10.0,15.0 and 24.0 h post-dosing for SudanⅠand SudanⅡ;whereas 1.0,2.0, 3.0,4.0,5.0,6.0,7.0,9.0,11.0,15.0,20.0,32.0 and 48.0 h post-dosing for Sudan III and Sudan IV) was collected immediately centrifuged and cleaned using Cleanert C mixed-mode polymeric sor-bent. Quantification was performed by an electrospray ionization source in the positive multiple reaction monitoring mode using D-SudanⅠas the internal standard compensated for any matrix effect variability, including extraction and ionization *** The pharmacokinetic results demonstrate that SudanⅠ,SudanⅡ,SudanⅢ,and SudanⅣreached the maximum point in the plasma drug concentration of rats at about 0.6046,1.362,4.196 and 4.341 h after oral administration,*** concentration decreased gradually with an elimination half-life(f) of 0.8374,1.8102,2.3909 and 2.364 h for SudanⅠ,SudanⅡ,SudanⅢ,and SudanⅣ,*** absorption rate constants(k) of SudanⅠ,SudanⅡ,SudanⅢ,and SudanⅣwere 3.996,1.393,0.4368 and 0.4395 1/h,which were significantly greater than their elimination rate constants(k) of 0.8277,0.3829,0.2899,and 0.2932 1/h,*** four Sudan dyes were easily absorb

关键词： pharmacokinetics Sudan dye Rat plasma UFLC-MS/MS multiple reaction monitoring

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A novel and validated liquid chromatography-tandem mass spectrometry method for analysis of hydrocortisone 17-butyrate in rabbit plasma and its skin penetration

A novel and validated liquid chromatography-tandem mass spec...

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中国药理学会第十一次全国学术会议

作者： ZHOU Zhi-ling~*,YANG Min~*,YU Xi-yong,CHEN Tie-feng,SHAN Zhi-xin,LIN Qiu-xiong, DENG Chun-yu,WU Yue-heng,LI Xiao-hong,ZHONG Shi-long,MAI Li-ping,LIN Shu-guang (Institute of Clinical Pharmacology,Guangdong Academy of Medical Sciences Medical Research Center of Guangdong General Hospital,Guangzhou 510080,China)

OBJECTIVE A novel,rapid and highly sensitive liquid chromatography-tandem mass spectrometry method(LC-MS /MS) was developed and validated for the determination and pharmacokinetic investigation of Hydrocortisone 17-Butyrate in rabbit plasma for the first *** Hydrocortisone 17-Butyrate and the internal standard(IS),Clobetasol Propionate,were extracted from plasma samples using solid phase extraction with Oasis HLB *** separation was performed on a Ultimat XB-C column(150 mm×4.6 mm i.d.,5 m particle size) using acetonitrile - water(30 mmol·L ammonium acetate buffer, 0.1%formic acid)(70:30,V/V) as the mobile phase at a flow rate of 0.8 ml·*** of Hydrocortisone 17-Butyrate and IS was achieved by tandem mass spectrometry with an electrospray ionization(ESI) interface in positive ion *** multiple reaction monitoring(MRM) using the transition of m/z 433.3→m/z 327.3 and m/z 467.2→m/z 373.2 was performed to quantify Hydrocortisone 17-Butyrate and the internal standard,*** healthy New Zea land white rabbits(4 males and 4 females) were applied 5g of cream containing 0.1%H-17-B to hairless skin area in the right back for 12 *** samples were col- lected before and at 1.0,2.0,3.0,4.0,6.0,8.0,10.0,12.0,24.0 and *** after drug *** AND CONCLUSION The calibration curves were linear over the range of 0.1 - 10 ng·ml with the lower limit of quantitation validated at 0.1 ng·ml.A typical regression equation was y=0.00826x -0.00229 with acorrelation coefficient(r) of 0.9997,where y represents the peak area ratio of H-17-B to that of IS and x represents the plasma concentration of *** intra- and inter-day precisions were within 13.10%,while the accuracy was within±7.20%of nominal *** three QC concentration levels 0.25,1.0 and 5.0ng·ml,the percent extraction recoveries of H-17-B obtained from plasma were(59.6±4.4)%,(63.1±7.6)%and (61.7±5.1)%,*** mean recovery for the inter

关键词： hydrocortisone 17-butyrate liquid chromatography-tandem mass spectrometry multiple reaction monitoring liquid-liquid extraction quantitative assay pharmacokinetics

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Selective and robust UPLC-MS/MS method for simultaneous quantitative determination of anlotinib, ceritinib and ibrutinib in rat plasma and its application to pharmacokinetic study

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中国药理学与毒理学杂志 2019年第10期 756-756页

作者： DU Ping GUAN Yin AN Zhuo-ling LI Peng-fei LIU Li-hong Beijing Chao-Yang Hospital Capital Medical University

OBJECTIVE A selective and robust ultrahigh performance liquid chromatography tandem mass spectrometry（UPLC-MS/MS） method has been firstly developed for the simultaneous determination of three nextgeneration anti-tumor tyrosine kinase inhibitors（anlotinib,ANL; ceritinib, CER; ibrutinib, IBR） in rat plasma using cost-effective protein precipitation extraction. METHODS and RESULTS LC separation was achieved on Waters XBrige C18 column（50 mm×2.1 mm, 3.5 μm） under gradient conditions in a run time of 5 min. Electrospray ionization in the positive ion mode was involved through mass spectrometry. multiple reaction monitoring（MRM） transitions were at m/z 408.2→339.2 for ANL, 558.2→433.2 for CER, 441.0→138.0 for IBR, 285.0→193.1 for diazepam（internal standard）, respectively. The optimized method was validated based on US FDA guideline, EMEA guideline as well as Pharmacopoeia of the People′s Republic of China. The assay was linear in the range of 0.1-20 μg·L-1for ANL, 2-1000 μg·L-1for CER, 1-500 μg·L-1for IBR. Intraand inter-day accuracy and precision for all analytes were ≦ 13.84% and ≦ 12.56%, respectively. ANL, CER and IBR were sufficiently stable under most investigated conditions. The optimized method was successful y applied for a pharmacokinetic study after single oral gavage administration of mixture（ANL, CER and IBR） at dose of 6, 25 and 10 mg·kg-1. CONCLUSION The proposed analytical assay demonstrates great improvements in respect of previous methods reported in literatures, such as costeffective sample preparation, short chromatographic time, smaller amount of sample（50 μL）, satisfied extraction recovery and matrix effect.

关键词： multiple reaction monitoring optimized method pharmacokinetic study

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