Objective: To establish a method for simultaneous determination of saikosaponin a, saikosaponin d, saikosaponin b1, saikosaponin b2 and saikosaponin k in Ruhe Neixiao liquids by UPLC-MS/MS. Methods: The samples were separated on a YMC-Triart C18 column (150 mm×2.1 mm, 3 μm) by gradient elution at a flow rate of 0.3 mL·min-1 using acetonitrile and 0.1% aqueous formic acid as the mobile phase. The column temperature was maintained at 35 ℃. Multiple reaction monitoring (SRM) scanning was employed for the quantification with switching electrospray ion (ESI) source polarity in negative mode. Results: The linear ranges of saikosaponin a, saikosaponin d, saikosaponin b1, saikosaponin b2 and saikosaponin k were 0.106-10.622 μg·mL-1 (r=0.999 6), 0.101-10.097 μg·mL-1(r=0.999 8), 0.098-9.840 μg·mL-1(r=0.999 9), 0.343-34.339 μg·mL-1(r=0.998 0) and 0.126-12.640 μg·mL-1(r=0.998 3), respectively. The average recoveries(n=6) were 98.6%(RSD=1.4%), 99.9%(RSD=1.2%), 101.1%(RSD=1.8%), 101.6%(RSD=1.8%) and 98.6%(RSD=1.9%), respectively. The content ranges of saikosaponin a, saikosaponin d, saikosaponin b1, saikosaponin b2 and saikosaponin k in Ruhe Neixiao liquids were 1.59-94.62 μg·mL-1, 0-0.52 μg·mL-1, 21.29-286.19 μg·mL-1, 14.78-156.64 μg·mL-1 and 0-66.01 μg·mL-1, respectively. Conclusion: The method can be used for simultaneous determination of saikosaponin a, saikosaponin d, saikosaponin b1, saikosaponin b2 and saikosaponin k in 25 samples from 10 manufacturers. This method is sensitive, accurate and reproducible, and provides a scientific reference for quality control and comprehensive evaluation of Ruhe Neixiao liquids.
ZHAO Yi-qing, WANG Yan-wei, YANG Yuan, ZHANG Hong-wei, WANG Xiao-yan
. Simultaneous determination of saikosaponin a, saikosaponin d, saikosaponin b1, saikosaponin b2 and saikosaponin k in Ruhe Neixiao liquids by UPLC-MS/MS*[J]. Chinese Journal of Pharmaceutical Analysis, 2023
, 43(10)
: 1702
-1708
.
DOI: 10.16155/j.0254-1793.2023.10.08
[1] 中华人民共和国药典 2020年版. 一部[S]. 2020: 304
ChP 2020. Vol Ⅰ[S]. 2020: 304
[2] 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
[3] 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]. 山西: 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]. Shanxi: Shanxi Provincial Institute of Traditional Chinese Medicine, 2021
[4] 刘亚雄, 罗卓雅, 乔莉, 等. 一种用于鉴别北柴胡与藏柴胡的方法及其应用: 中国, CN 112782320A[P]. 2021-05-11
LIU YX, LUO ZY, QIAO L, et al. A Kind of Method for Distinguishing B. marginatum var. stenophyllum and B. chinense DC. and Its Application: China, CN112782320A[P]. 2021-05-01
[5] 欧小龙, 黄涛阳. 柴胡属植物化学成分研究进展[J]. 中药材, 2021, 44(3):749
OU XL, HUANG TY. Advances on the studies of chemical constituents of Bupleurum L.[J]. J Chin Med Mater, 2021, 44(3):749
[6] 李军, 姜华, 张延萍, 等. 柴胡中酰化柴胡皂苷的含量测定[J]. 中国药学杂志, 2015, 50(8):722
LI J, JIANG H, ZHANG YP, et al. Determination of acyl-saikosaponin in Radix Bupleuri[J]. Chin Pharm J, 2015, 50(8):722
[7] 李力恒, 陈丽萍, 胡晓阳, 等. 柴胡的化学成分及药理作用研究进展[J]. 中医药学报, 2023, 51(2):109
LI LH, CHEN LP, HU XY, et al. Advance on the chemical and pharmacological effects studies of Radix Bupleuri[J]. Acta Chin Med Pharmacol, 2023, 51(2):109
[8] 夏召弟, 刘霞. 北柴胡化学成分及质量控制方法研究进展[J]. 中国现代中药, 2021, 23(5):940
XIA ZD, LIU X. Research progress on chemical composition and quality control methods of Bupleurum chinense[J]. Mod Chin Med, 2021, 23(5):940
[9] 成睿珍, 张春艳. 柴胡皂苷类药理活性的研究进展[J]. 职业与健康, 2021, 37(4):568
CHNEG RZ, ZHANG CY. Research progress on pharmacological activities of saikosaponins from Radix Bupleurum[J]. Occup Health, 2021, 37(4):568
[10] 陈晶, 傅欣彤, 陈有根, 等. 基于UHPLC-QE Plus-MS/MS法分析柴黄颗粒及柴胡中化学成分[J]. 中草药, 2022, 53(15):4634
CHEN J, FU XT, CHEN YG, et al. Analysis of chemical constituents of Chaihuang granules by UHPLC-QE Plus-MS/MS[J]. Chin Tradit Herb Drugs, 2022, 53(15):4634
[11] 闵宇航, 王京辉, 范妙璇, 等. 柴胡饮片皂苷类成分变化及质量控制研究[J]. 药物分析杂志, 2014, 34(5):836
MIN YH, WANG JH, FAN MX, et al. Study on the variation of saikosaponins and the quality control of the decoction pieces of Radix Bupleuri[J]. Chin J Pharm Anal, 2014, 34(5):836
[12] 李军, 姜华, 张延萍, 等. 单味柴胡煎煮过程中皂苷煎出量的变化[J]. 中国实验方剂学杂志, 2013, 24(6):602
LI J, JIANG H, ZHANG YP, et al. Content change of saikosaponins during preparation of saiko decoction[J]. Chin J Exp Tradit Med Form, 2013, 24(6):602
[13] 刘树强, 王术玲, 高晓玲, 等. 柴胡水煎过程中皂苷成分的变化规律[J]. 中国新药与临床药理, 2013, 24(6):602
LIU SQ, WANG SL, GAO XL, et al. Variation of saponins in Radix Bupleuri during decoction process[J]. Tradit Chin Drug Res Clin Pharmacol, 2013, 24(6):602
[14] 霍务贞, 卫世杰. HPLC法测定感冒清口服液中柴胡皂苷a、d的含量[J]. 中国药房, 2013, 24(8):741
HUO WZ, WEI SJ. Content determination of saikosaponin a and saikosaponin d in Ganmaoqing oral liquid by HPLC[J]. China Pharm, 2013, 24(8):741
[15] 卫昊, 刘清, 卫伟光, 等. HPLC法测定秦岭柴胡及其不同提取物中柴胡皂苷a和柴胡皂苷d[J]. 中成药, 2013, 35(2):342
WEI H, LIU Q, WEI WG, et al. Determination of saikosaponin a, d in different extracts of Bupleurum longicaule Wall. ex DC. var. giraldii Wolff by HPLC[J]. Chin Tradit Pat Med, 2013, 35(2):342
[16] 刘潇潇, 罗卓雅, 计周正, 等. 小柴胡颗粒制剂及其中草药原料中藏柴胡掺伪的检测方法与流程: 中国, CN201910909112[P]. 2020-02-11
LIU XX, LUO ZY, JI ZZ, et al. Detection Method and Process of B. marginatum var. stenophyllum Adulteration in Xiaochaihu Granule Preparation and Its Chinese Herbal Medicine Raw Materials: China, CN201910909112[P]. 2020-02-11
