安全监测

超高效液相色谱-三重四极杆质谱法检测柴胡中藏柴胡的掺伪*

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  • 1.甘肃省药品检验研究院,兰州 730030;
    2.甘肃省药品监督管理局审核查验中心,兰州 730030;
    3.北京葵花医药研究有限责任公司,北京 100050
第一作者 李 敏 Tel:18809421680;E-mail:1781722359@qq.com
李 婷 Tel:13693527343;E-mail:1006287965@qq.com
** 张 平 Tel:17709310037;E-mail:58735870@qq.com
杨玲霞 Tel:13909427927;E-mail:yanglingxia009@126.com

修回日期: 2024-04-09

  网络出版日期: 2024-08-07

基金资助

* 甘肃省药品监督管理局,中药材及饮片质量控制重点实验室(2023GSMPA-KL06);国家药监局中药材及饮片质量控制重点实验室项目(2021GSMPA-KL04,2022GSMPA-KL12,2022GSMPA-KL10,2020GSMPA-KL15);甘肃省药品监督管理局,甘肃省中药饮片炮制规范化研究(2022GSMPA-0075)

Determination of adulteration of Bupleurum marginatum var. stenophyllum in Bupleurum by UPLC-QqQ-MS*

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  • 1. Gansu Institute for Drug Control, Lanzhou 730030, China;
    2. Center for Inspection of GSMPA, Lanzhou 730030, China;
    3. Beijing Sunflower Pharmaceutical Research Co.,Ltd., Beijing 100050, China

Revised date: 2024-04-09

  Online published: 2024-08-07

摘要

目的: 建立检测柴胡及藏柴胡中柴胡皂苷K成分的液相色谱-质谱法(LC-MS)检查方法,用以快速鉴别北柴胡是否为藏柴胡或混有藏柴胡。同时对16批藏柴胡和157批柴胡饮片中的柴胡皂苷K进行检测。方法: 采用超高效液相色谱-三重四极杆串联质谱(UPLC-QqQ-MS)对柴胡及藏柴胡中柴胡皂苷K进行检测,色谱柱为Phenomenex Kinetex C18(100 mm×2.1 mm,1.7 μm),流动相为乙腈(A)-水(B),梯度洗脱(0~5 min,15%A→25%A;5~30 min,25%A→30%A;30~35 min,30%A→90%A;35~36 min,90%A→15%A;36~40 min,15%A),流速0.3 mL·min-1,柱温25 ℃,进样量5 μL;采用电喷雾离子源(ESI-),负离子模式扫描,多反应监测(MRM)模式检测,选择柴胡皂苷K特征分子离子峰m/z 943.5→797.3、m/z 943.5→635.3和m/z 943.5→781.3作为检测离子对。结果: 16批藏柴胡中柴胡皂苷K的量远高于限度要求,157批柴胡饮片中有8批样品中均检出藏柴胡类成分柴胡皂苷K。结论: 所建立的方法经方法学验证,专属性强,以期制定柴胡中藏柴胡成分检查项补充检验方法,提升柴胡饮片质量控制标准及真伪鉴别研究,可进一步有效控制其质量,保障临床疗效。

本文引用格式

李敏, 李婷, 韩潇潇, 马潇, 李冬华, 张平, 杨玲霞 . 超高效液相色谱-三重四极杆质谱法检测柴胡中藏柴胡的掺伪*[J]. 药物分析杂志, 2024 , 44(6) : 999 -1008 . DOI: 10.16155/j.0254-1793.2024.06.10

Abstract

Objective: To establish a liquid chromatography mass spectrometry (LC-MS) method for the detection of nepasaikosaponin K in Bupleurum marginatum var. stenophyllum, which could be used to quickly identify whether Bupleurum marginatum var. stenophyllum was substituted for Bupleurum or was mixed with Bupleurum. At the same time, nepasaikosaponin K was detected in 16 batches of Bupleurum marginatum var. stenophyllum and 157 batches of bupleurum decoction pieces. Methods: Ultra-high performance liquid chromatography (UPLC) coupled with triple quadruple mass spectrometry (QqQ MS) was used to detect nepasaikosaponin K in Bupleurum and Bupleurum marginatum var. stenophyllum. Determination was carried out with the application of a Phenomenex Kinetex C18 (2.1 mm×100 mm, 1.7 μm) column at temperature of 25 ℃. The mobile phase was composed of acetonitrile(A) and water(B) with gradient elution(0-5 min 15%A→25%A;5-0 min,25%A→30%A; 30-35 min,30%A→90%A;35-36 min,90%A→15%A;36-40 min,15%A)at a flow rate of 0.3 mL·min-1. The electrospray ionization(ESI-) source was performed in multiple reaction monitoring(MRM)mode of the transitions of m/z 943.5→797.3, m/z 943.5→635.3, and m/z 943.5→781.3. Results: The contents of nepasaikosaponin K detected in 16 batches of Bupleurum marginatum var. stenophyllum were much higher than minimum requirements. Nepasaikosaponin K was detected in 8 out of 157 batches of Bupleurum. Conclusion: The established method is verified by methodology to be specific, so as to develop a supplementary test method for the components of Bupleurum and Bupleurum marginatum var. stenophyllum. to improve the quality control standard and authentic identification investigation, and to effectively control the quality of Bupleurum decoction pieces and guarantee its clinical efficacy.

参考文献

[1] 颜美玲,杨柳,侯阿娇,等. 柴胡化学成分及药理作用研究进展[J]. 中医药信息, 2018, 35(5): 103
YAN ML, YANG L, HOU AJ, et al. Research progress on chemical composition and pharmacological effect of Bupleurum chinense DC.[J]. Inf Tradit Chin Med, 2018, 35(5): 103
[2] 郭泰麟, 康廷国, 张慧. 不同产地南北柴胡中柴胡皂苷的含量测定[J]. 天津中医药大学学报, 2020, 39(2): 221
GUO TL, KANG TG, ZHANG H. Determination of saikosaponin in Bupleurum chinense DC. and Bupleurum scorzonerifolium Willd from different areas[J]. Tianjin Univ Tradit Chin Med, 2020, 39(2): 221
[3] 林家冉, 赵林华, 邸莎, 等. 柴胡的临床应用及其用量探究[J]. 吉林中医药, 2019, 39(4): 449
LIN JR, ZHAO LH, DI S, et al. Exploration about the clinical application and dosage of Bupleurum[J]. Jilin J Chin Med, 2019, 39(4): 449
[4] 赵佳琛, 翁倩倩, 张悦, 等. 经典名方中柴胡药材的本草考证[J]. 中国中药杂志, 2020, 45(3): 697
ZHAO JC, WENG QQ, ZHANG Y, et al. Textual research on Bupleuri radix in Chinese classical prescriptions[J]. Chin J Chin Mater Med, 2020, 45(3): 697
[5] 李艳凤, 刘雅舒, 李艳生. 柴胡的化学成分与药理作用研究进展[J]. 西北药学杂志, 2022, 37(5): 186
LI YF, LIU YS, LI YS. Chemical composition and pharmacological effects of Bupleuri radix [J]. North West Pharm J, 2022, 37(5): 186
[6] 徐雪娇, 李天英, 李欣, 等. 柴胡化学成分及抗抑郁机制研究进展[J]. 化学工程师, 2022, 36(6): 65
XU XJ, LI TY, LI X, et al. Research progress on the chemical constituents and antidepressant mechanism of Bupleurum[J]. Chem Eng, 2022, 36(6): 65
[7] 黄冬芳, 韦金玉, 梁洁, 等. 柴胡质量标志物的预测分析[J]. 中华中医药学刊, 2021, 39(10): 126
HUANG DF, WEI JY, LIANG J, et al. Prediction and analysis of Chaihu(Bupleurum Chinense DC.) on quality marker[J]. Chin Arch Tradit Chin Med, 2021, 39(10): 126
[8] 吴丹, 高耀, 向欢, 等. 基于网络药理学的柴胡抗抑郁作用机制研究[J]. 药学学报, 2018, 53(2): 210
WU D, GAO Y, XIANG H, et al. Exploration into mechanism of antidepressant of Bupleuri radix based on network pharmacology[J]. Acta Pharm Sin, 2018, 53(2): 210
[9] ASHOUR ML, WINK M. Genus Bupleurum: a review of its phytochemisty, pharmacology and modes of action[J]. J Pharm Pharmcol, 2011, 63(3):305
[10] 李春娜, 刘悦, 刘洋洋, 等. 北柴胡化学成分及活性部位研究进展[J]. 中华中医药学刊, 2014, 32(11): 2674
LI CN, LIU Y, LIU YY, et al. Advances in research of chemical constituents and active constituents of Dictamnus dasycarpus DC.[J]. Chin Arch Tradit Chin Med, 2014, 32(11): 2674
[11] 高丽萍. 柴胡有效成分与药理作用探究[J]. 临床医药文献电子杂志, 2017, 70(4): 13853
GAO LP. Study on the effective components and pharmacological activity of Bupleurum chinense DC.[J]. Elect J Clin Med Liter, 2017, 70(4): 13853
[12] 贾为壹, 刘佳佳, 胡睿, 等. 小柴胡颗粒激活Nrf2通路抗TAA致大鼠急性肝损伤的机制探讨[J]. 中国实验方剂学杂志, 2019, 25(8): 5459
JIA WY, LIU JJ, HU R, et al. Therapeuticmechanism of Xiaochaihu granule on acute liver injury induced by thioacetamide in rats through Nrf2 pathway[J]. Chin J Exp Tradit Med Form, 2019, 25(8): 5459
[13] 梁镇标, 刘力, 晁志. 柴胡属植物资源及生产状况调查[J]. 时珍国医国药, 2012, 23(8): 2011
LIANG ZB, LIU L, CHAO Z. Investigation of medicinal Bupleurum resources and current situation of Chaihu production[J]. Lishizhen Med Mater Med Res 2012, 23(8): 2011
[14] 严华, 董亚娟, 程显隆, 等. 南柴胡与常见混伪品的鉴别方法研究[J]. 中国药学杂志, 2015, 50(2): 109
YAN H, DONG YJ, CHENG XL, et al. Identification of Bupleurum scorzonerifolium and its adulterants[J]. Chin Pharm J, 2015, 50(2): 109
[15] 赖晶, 史中飞, 宋平顺, 等. 基于ITS序列位点特异性PCR鉴别北柴胡掺伪藏柴胡[J]. 现代中药研究与实践, 2021, 35(2): 18
LAI J, SHI ZF, SONG PS, et al. Identification of Bupleurum marginatum var. stenophyllum adulterated Bupleurum chinense DC. by PCR amplification of based on ITS sequences[J]. Res Pract Chin Med, 2021, 35(2): 18
[16] 王梦迪, 靳光乾. 柴胡中药资源研究进展[J]. 山东林业科技, 2019, 49(3): 107
WANG MD, JIN GQ. Research progress on the pesources of Bupleurum chinensis [J]. Shan dong Forestry Sci Technol, 2019, 49(3): 107
[17] 王砚. 竹叶柴胡和北柴胡品质比较研究[D]. 成都:成都中医药大学, 2014
WANG Y. Comparative Study on the Quality of B. marginatum Wall. ex DC. and Bupleurem chinense DC.[D]. Chengdu: Chengdu University of Tradittion Chinese Medcine, 2014
[18] 郭佳琪, 杨印军, 方伟, 等. 藏柴胡以及种植北柴胡和竹叶柴胡的皂苷含量研究[J]. 中国现代中药, 2018, 20(1): 34
GUO JQ, YANG YJ, FANG W, et al. Saikosaponins content in Bupleurum marginatum var. stenophyllum and cultivated B. chinese and B. marginatum[J]. Mod Chin Med, 2018, 20(1): 34
[19] 魏晓萌. 锥叶柴胡化学成分及质量控制方法研究[D]. 北京:北京中医药大学, 2018
WEI XM. Study on Chemical Composition and Quality Control of Bupleurum bicaule Helm[D]. Beijing: Beijing University of Chinese Medicine, 2018
[20] 严华, 董亚娟, 程显隆, 等. 南柴胡与常见混伪品的鉴别方法研究[J]. 中国药学杂志, 2015, 50(2): 109
YAN H, DONG YJ, CHENG XL, et al. Identification of Bupleurum scorzonerifolium and its adulterants[J]. Chin Pharm J, 2015, 50(2): 109
[21] 丁锤, 徐莹, 马孝熙, 等. 柴胡属5种易混药材的鉴别研究[J]. 中药材, 2016, 39(9): 1975
DING C, XU Y, MA XX, et al. Identification on five kinds of easily confused Bupleurum medicinal materials[J]. J Chin Med Mater, 2016, 39(9): 1975
[22] 王惠, 刘霞. 藏柴胡的研究进展[J]. 世界最新医学信息文摘, 2019, 19(20): 110
WANG H, LIU X. Research progress on Bupleurum marginatum var. stenophyllum[J]. World Latest Med Inf, 2019, 19(20): 110
[23] 孙旖.中药柴胡与常见混伪品的鉴别方法分析[J]. 光明中医, 2018, 33(17): 2502
SUN Y. Analysis of the identification method of traditional Chinese medicine Bupleuri radix and common adulterants[J]. Guangming J Chin Med, 2018, 33(17): 2502
[24] 夏召弟. 藏柴胡与北柴胡化学成分及质量控制方法的比较研究[D]. 太原: 山西省中医药研究院, 2021
XIA ZD. Comparative Study on Chemical Constituents and Quality Control Methods of B. marginatum var. stenophyllum and B. chinense DC. [D]. Taiyuan: Shanxi Provincial Institute of Traditional Chinese Medicine, 2021
[25] 赵丹彤, 高一军, 毕天琛, 等. 感冒清热颗粒中藏柴胡掺伪检测方法的建立及掺伪限度拟定[J]. 中国药房, 2022, 33(20): 2454
ZHAO DT, GAO YJ, BI TC, et al. Establishment of the detection method for the adulteration of Bupleurum marginatum in Ganmao Qingre granules and determination of adulteration limit[J]. J Chin Pharm, 2022, 33(20): 2454
[26] 赵丹彤, 高一军, 毕天琛, 等. 柴胡属饮片中藏柴胡掺伪检测方法研究[J]. 药学研究, 2022, 41(10): 653
ZHAO DT, GAO YJ, BI TC, et al. Analytical method of Bupleurum marginatunm var. stenophyllum sdulteration in Bupleurum[J]. J Pharm Res, 2022, 41(10): 653
[27] 郭佳琪, 杨印军, 方伟, 等. 柴胡以及种植北柴胡和竹叶柴胡的皂苷含量研究[J]. 中国现代中药, 2018, 20(1): 34
GUO JQ, YANG YJ, FANG W, et al. Saikosaponins content in Bupleurum marginatum var. stenophyllum and cultivated B. chinese and B. marginatum[J]. Mod Chin Med, 2018, 20(1): 34
[28] 张军, 苏本正,戴衍朋, 等. 基于市售柴胡饮片质量考察的质量控制标准提升及真伪鉴别研究[J]. 中华中医药杂志, 2021, 36(10): 6172
ZHANG J, SU BZ, DAI YP, et al. Study on improvement of quality control standard and true and false identification based on quality investigation of commercial Bupleuri radix pieces[J]. Chin Med Pharm, 2021, 36(10): 6172
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