A sensitive LC-MS/MS method for simultaneous assay of three iridiods in Gardenia jasminoides Ellis
-
摘要: 目的 建立同时测定栀子中3种环烯醚萜苷类成分含量的方法。 方法 采用液相色谱-串联质谱（LC-MS/MS）法。色谱条件：Dikma Diamonsil® C18柱（100 mm×4.6 mm，5 μm）；流动相为0.1%乙酸水（A）-0.1%乙酸乙腈（B），梯度洗脱；流速为0.4 ml/min；柱温40℃；进样量2 μl。质谱条件：电喷雾离子化电离源（ESI），正/负离子检测，雾化气流量3 L/min，干燥气流量15 L/min，脱溶剂管温度240℃，加热块温度400℃，碰撞气压力230 kPa，以多反应监测模式（MRM）配对离子方式进行定量，山栀苷、京尼平龙胆双糖苷、栀子苷选择的离子对质荷比分别为m/z 391.10→149.30，m/z 573.40→365.05，m/z 447.30→225.15。 结果 回归方程为：山栀苷Y=243.810X-289.957，r=0.999 9；京尼平龙胆双糖苷Y=137.125X+2 092.76，r=0.999 6；栀子苷Y=2 030.32X+823 213，r=0.999 8；线性范围分别为10.76~2 152 ng/ml、516~4 128 ng/ml、2 000~20 000 ng/ml。精密度、稳定性、重复性和加样回收率试验结果均符合要求。 结论 此方法可快速、准确、灵敏地测定栀子中3种环烯醚萜苷类成分的含量，为栀子的质量控制提供依据。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.
-
Key words:
- Gardenia jasminoides Ellis /
- shanzhiside /
- genipin-1-gentiobioside /
- geniposide /
- LC-MS/MS
-
[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. 期刊类型引用(7)
1. 李睿，张莹莹，刘卫红，宋艳秋，李龙星，李海峰. 相同产地3种龙胆属植物根及根茎中化学成分的差异分析. 中国药房. 2023(03): 303-308 . 
百度学术2. 阿润，王秀兰，策力木格，王徽. 基于网络药理学红花三味散治疗非酒精性脂肪肝病的作用机制. 医药导报. 2021(05): 622-630 . 百度学术3. 林敏. HPLC-MS/MS法同时测定丹栀逍遥丸中六个成分的含量. 海峡药学. 2021(12): 74-78 . 百度学术4. 王博，张婧，吴剑平，严凤. 液相色谱-串联质谱法测定植物提取物的研究进展. 食品安全质量检测学报. 2020(15): 4973-4980 . 百度学术5. 徐鑫，戚华文，高德嵩，蔡新娜，金磊，金红利，王超然，刘艳芳，梁鑫淼. 基于化学模式识别的栀子UPLC定量指纹图谱研究. 中国中药杂志. 2020(18): 4416-4422 . 百度学术6. Ruirui Chang，Jialin Liu，Yusha Luo，Taohong Huang，Qiang Li，Jun Wen，Weidong Chen，Tingting Zhou. Isoflavones' effects on pharmacokinetic profiles of main iridoids from Gardeniae Fructus in rats. Journal of Pharmaceutical Analysis. 2020(06): 571-580 . 必应学术7. 王小庆. 药用植物双参中环烯醚萜类. 临床医药文献电子杂志. 2019(64): 173+177 . 百度学术其他类型引用(5)
-
点击查看大图
计量
- 文章访问数: 4726
- HTML全文浏览量: 467
- PDF下载量: 412
- 被引次数: 12
下载:
