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Volume 37 Issue 1
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Article Navigation >  Journal of Pharmaceutical Practice and Service  > 2019  >  37(1): 19-22

CHANG Ruirui, CHEN Weidong, ZHOU Tingting. A sensitive LC-MS/MS method for simultaneous assay of three iridiods in Gardenia jasminoides Ellis[J]. Journal of Pharmaceutical Practice and Service, 2019, 37(1): 19-22. doi: 10.3969/j.issn.1006-0111.2019.01.005
Citation: CHANG Ruirui, CHEN Weidong, ZHOU Tingting. A sensitive LC-MS/MS method for simultaneous assay of three iridiods in Gardenia jasminoides Ellis[J]. Journal of Pharmaceutical Practice and Service, 2019, 37(1): 19-22. doi: 10.3969/j.issn.1006-0111.2019.01.005
shu

A sensitive LC-MS/MS method for simultaneous assay of three iridiods in Gardenia jasminoides Ellis

doi: 10.3969/j.issn.1006-0111.2019.01.005
  • 1.

    School of Pharmacy, Anhui University of Chinese Medicine, Hefei 233000, China;Department of Pharmaceutical Analysis, School of Pharmacy, Naval Medical University, Shanghai 200433, China

  • 2.

    School of Pharmacy, Anhui University of Chinese Medicine, Hefei 233000, China

  • 3.

    Department of Pharmaceutical Analysis, School of Pharmacy, Naval Medical University, Shanghai 200433, China

  • Received Date: 2018-10-17
  • Rev Recd Date: 2018-11-23
  • Objective To develop a simple, rapid and sensitive method for the determination of major compounds from Gardenia jasminoides Ellis using liquid chromatography tandem mass spectrometry (LC-MS/MS). Methods The analysis was performed on Dikma Diamonsil® C18(100 mm×4.6 mm, 5 μm)column with acetonitrile -0.1% acetic acid and 0.1% acetic acid-water as mobile phase at a rate of 0.4 ml/min.The column temperature was set at 40℃ and the injection volume was 2 μl.Quantification of these compounds was performed by LC-MS/MS with positive or negative ion mode electrospray ionization (ESI) in the multiple reaction monitoring (MRM) mode.Nebulizer gas, 3 L/h; drying gas, 15 L/h; desolvation line (DL) temperature, 240℃; heat block temperature, 300℃; CID, 230 kPa.The mass transition of the precursor/product ions was monitored at m/z 391.10→149.30 for shanzhiside, 573.40→365.05 for genipin-1-gentiobioside, 447.30→225.15 for geniposide. Results The regress equation of shanzhiside, genipin-1-gentiobioside and geniposide were Y=243.810X-289.957, r=0.999 9; Y=137.125X + 2 092.76, r=0.999 6; Y=2 030.32X+823 213, r=0.999 8 in the range of 10.76-215.2 ng/ml; 516-4 128 ng/ml; 2 000-20 000 ng/ml respectively.This validated method has good repeatability, precision, recovery and stability.The results meet the requirements by regulation. Conclusion This method shortened the analysis time and improved efficiency.It assayed the three iridoid glycosides in Gardenia jasminoides Ellis sensitively and precisely.This method can be used for the quality control of Gardenia jasminoides Ellis.
  • [1] 国家药典委员会.中华人民共和国药典2015年版(一部)[M].北京:中国医药科技出版社,2015.
    [2] LIU H,CHEN Y F,LI F,et al.Fructus Gardenia (Gardenia jasminoides J.Ellis) phytochemistry,pharmacology of cardiovascular,and safety with the perspective of new drugs development[J].J Asian Nat Prod Res,2013,15(1):94-110.
    [3] XING H,ZHANG K,ZHANG R,et al.Antidepressant-like effect of the water extract of the fixed combination of Gardenia jasminoides,Citrus aurantium and Magnolia officinalis in a rat model of chronic unpredictable mild stress[J].Phytomedicine,2015,22(13):1178-1185.
    [4] WANG X,WANG G C,RONG J,et al.Identification of steroidogenic components derived from Gardenia jasminoides Ellis potentially useful for treating postmenopausal syndrome[J].Front Pharmacol,2018,9:390.
    [5] HAN Y,WEN J,ZHOU T,et al.Chemical fingerprinting of Gardenia jasminoides Ellis by HPLC-DAD-ESI-MS combined with chemometrics methods[J].Food Chem,2015,188:648-657.
    [6] 郭建华,田成旺,刘晓,等.中药环烯醚萜类化合物研究进展[J].药物评价研究,2011,34(4):293-297.
    [7] 刘武占,范建伟,高艳红,等.HPLC同时测定栀子中8个环烯醚萜苷类成分的含量[J].中国中药杂志,2012,37(16):2417-2421.
    [8] 关皎,朱鹤云,李菁,等.UFLC法同时测定栀子中4种活性成分的含量[J].中药新药与临床药理,2017,2(28):219-222.
    [9] CORAN S A,MULAS S,VASCONI A.Profiling of components and validated determination of iridoids in Gardenia Jasminoides Ellis fruit by a high-performance-thin-layer-chromatography/mass spectrometry approach[J].J Chromatogr A,2014,1325(2):221-226.
    [10] 霍江燕,梁生旺.中药复方LC-MS技术研究进展[J].亚太传统医药,2015,11(24):60-62.
    [11] JIANG P,MA Y,GAO Y,et al.A comprehensive evaluation of the metabolism of genipin-1-β-D-gentiobioside in vitro and in vivo by using HPLC-Q-TOF[J] J Agric Food Chem,2016,64(27):5490-5498.
    [12] WANG L,LIU S,ZHANG X,et al.A strategy for identification and structural characterization of compounds from Gardenia jasminoides by integrating macroporous resin column chromatography and liquid chromatography-tandem mass spectrometry combined with ion-mobility spectrometry[J].J Chromatogr A,2016,1452:47-57.
    [13] 张建花,许月明,何玉琼,等.巴戟天环烯醚萜苷类成分含量测定和提取方法的研究[J].药学实践杂志,2017,35(4):328-333.
    [14] WU H,LI X,YAN X,et al.An untargeted metabolomics-driven approach based on LC-TOF/MS and LC-MS/MS for the screening of xenobiotics and metabolites of Zhi-Zi-Da-Huang decoction in rat plasma[J].J Pharm Biomed Anal,2015,115:315-322.
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A sensitive LC-MS/MS method for simultaneous assay of three iridiods in Gardenia jasminoides Ellis

doi: 10.3969/j.issn.1006-0111.2019.01.005
  • 1. School of Pharmacy, Anhui University of Chinese Medicine, Hefei 233000, China;Department of Pharmaceutical Analysis, School of Pharmacy, Naval Medical University, Shanghai 200433, China
  • 2. School of Pharmacy, Anhui University of Chinese Medicine, Hefei 233000, China
  • 3. Department of Pharmaceutical Analysis, School of Pharmacy, Naval Medical University, Shanghai 200433, China
  • Received Date: 2018-10-17
  • Rev Recd Date: 2018-11-23

Abstract: Objective To develop a simple, rapid and sensitive method for the determination of major compounds from Gardenia jasminoides Ellis using liquid chromatography tandem mass spectrometry (LC-MS/MS). Methods The analysis was performed on Dikma Diamonsil® C18(100 mm×4.6 mm, 5 μm)column with acetonitrile -0.1% acetic acid and 0.1% acetic acid-water as mobile phase at a rate of 0.4 ml/min.The column temperature was set at 40℃ and the injection volume was 2 μl.Quantification of these compounds was performed by LC-MS/MS with positive or negative ion mode electrospray ionization (ESI) in the multiple reaction monitoring (MRM) mode.Nebulizer gas, 3 L/h; drying gas, 15 L/h; desolvation line (DL) temperature, 240℃; heat block temperature, 300℃; CID, 230 kPa.The mass transition of the precursor/product ions was monitored at m/z 391.10→149.30 for shanzhiside, 573.40→365.05 for genipin-1-gentiobioside, 447.30→225.15 for geniposide. Results The regress equation of shanzhiside, genipin-1-gentiobioside and geniposide were Y=243.810X-289.957, r=0.999 9; Y=137.125X + 2 092.76, r=0.999 6; Y=2 030.32X+823 213, r=0.999 8 in the range of 10.76-215.2 ng/ml; 516-4 128 ng/ml; 2 000-20 000 ng/ml respectively.This validated method has good repeatability, precision, recovery and stability.The results meet the requirements by regulation. Conclusion This method shortened the analysis time and improved efficiency.It assayed the three iridoid glycosides in Gardenia jasminoides Ellis sensitively and precisely.This method can be used for the quality control of Gardenia jasminoides Ellis.

CHANG Ruirui, CHEN Weidong, ZHOU Tingting. A sensitive LC-MS/MS method for simultaneous assay of three iridiods in Gardenia jasminoides Ellis[J]. Journal of Pharmaceutical Practice and Service, 2019, 37(1): 19-22. doi: 10.3969/j.issn.1006-0111.2019.01.005
Citation: CHANG Ruirui, CHEN Weidong, ZHOU Tingting. A sensitive LC-MS/MS method for simultaneous assay of three iridiods in Gardenia jasminoides Ellis[J]. Journal of Pharmaceutical Practice and Service, 2019, 37(1): 19-22. doi: 10.3969/j.issn.1006-0111.2019.01.005
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