UPLC-MS/MS法测定舒肝丸中川楝素的含量

目的：建立UPLC-MS/MS 定量测定舒肝丸中川楝素含量的分析方法。方法：采用Acquity UPLC BEH C₁₈色谱柱（2.1 mm×50 mm，1.7 mm），以乙腈-0.01% 甲酸溶液为流动相进行等度洗脱，流速0.35 mL·min^-1，质谱使用电喷雾电离源（ESI）负离子模式，多反应检测（MRM）扫描方式检测，分析时间3.5 min。结果：川楝素质量浓度在1.115~1 115 ng·mL^-1 范围内线性关系良好（r=0.999 9）；平均加样回收率（n=9）为99.0%。21 批舒肝丸样品中川楝素含量为2.40~40.0 μg·g^-1。结论：本法可推荐用于舒肝丸中川楝素的含量测定标准制定。

Objective: To establish an UPLC-MS/MS method for determination of toosendanin in Shugan pills. Methods: The analysis was performed on an Acquity UPLC BEH C₁₈ column(2.1 mm×50 mm,1.7 mm)with acetonitrile and 0.01% formic acid as mobile phase at a flow rate of 0.35 mL·min^-1. The mass spectrometer was operated in the positive ioization electrospray mode using multiple reaction monitoring(MRM)for analysis of toosendanin. Results: The linear range of toosendanin was 1.115-1 115 ng·mL^-1(r=0.999 9)and the average recovery(n=9)was 99.0%. The content range of toosendanin in 21 batches of Shugan pills was 2.40-40.0 μg·g^-1. Conclusion: The method was recommended to be used to formulate the assay standard of toosendanin in Shugan pills.

[1] 中国药典2015 年版. 一部[S]. 2015:1600 ChP 2015. Vol Ⅰ[S]. 2015:1600
[2] 李志敏,左新,王兆炜,等. 川楝素驱猪蛔虫体外杀虫试验研究[J]. 中国兽药杂志,2008,42(3):28 LI ZM,ZUO X,WANG ZW,et al. Studies on the effects of toosendanin on ascaris sum in vitro[J]. Chin J Vet Med,2008,42 (3):28
[3] WATANABE T,SAKAMOTO N,NAKAGAWA M,et al. Inhibitory effect of a triterpenoid compound,with or without alpha interferon, on hepatitis C virus infection[J]. Antimicrob Agents Chemother, 2011,55(6):2537
[4] 齐双岩,熊彦红,金若敏. 川楝子致小鼠肝毒性时效、量效关系研 究[J]. 时珍国医国药,2008,19(11):2694 QI SY,XIONG YH,JIN RM. Time-dose-effect studies on hepatotoxicity of mice induced by Fructus Toosendan[J]. Lishizhen Med Mater Med Res,2008,19(11):2694
[5] 张先福,王建华,张树方,等. 川楝素对昆明小鼠的胚胎毒性研究[J]. 畜牧兽医学报,2005,36(3):301 ZHANG XF,WANG JH,ZHANG SF,et al. Research of embryotoxicity of toosendanin in Kunming mice[J]. Acta Vet Zootech Sin,2005,36(3):301
[6] 周乐华,李迎春,窦志英. 川楝子及其炮制品中川楝素含量测定 研究[J]. 天津药学,2011,23(1):20 ZHOU LH,LI YC,DOU ZY. Determination of toosendanin in processed products of Toosendan Fructus[J]. Tianjin Pharm,2011, 23(1):20
[7] 陈强,周浓,王荣繁. HPLC 测定川楝子不同采收期及不同部位中 川楝素的含量[J]. 资源开发与市场,2012,28(9):777 CHEN Q,ZHOU N,WANG RF. Determination of toosendanin in different parts of Melia toosendan in different seasons by HPLC[J]. Resour Dev Mark,2012,28(9):777
[8] 李洁玉,沈力,周浓,等. HPLC 测定不同来源川楝子中川楝素[J]. 光谱实验室,2013,30(1):294 LI JY,SHEN L,ZHOU N,et al. Determination of toosendanin in different sources of Melia toosendan by HPLC[J]. Chin J Spectrosc Lab,2013,30(1):294
[9] 张烨,周浓,夏从龙. HPLC 测定妇乐颗粒中川楝素含量[J]. 辽 宁中医药大学学报,2010,12(4):220 ZHANG Y,ZHOU N,XIA CL. Quantitative determination of toosendanin in Fule Keli by HPLC[J]. J Liaoning Univ TCM, 2010,12(4):220
[10] 罗文汇,毕晓黎,孙冬梅. LC-MS 法测定川楝子中川楝素[J]. 中 成药,2014,36(7):1556 LUO WH,BI XL,SUN DM. Determination of toosendanin in Toosendan Fructus by LC-lus[J]. Chin Tradit Pat Med,2014,36 (7):1556
[11] 吴忠杰. 超高效液相色谱-质谱联用法测定川楝子中川楝素的 含量[J]. 世界中西医结合杂志,2015,10(7):940 WU ZJ. Determination of toosendanin content in Toosendan Fruit by UPLC/MS[J]. World J Integr Tradit West Med,2015,10(7):940
[12] 吕桌,张明,王莉,等. HPLC-MS/MS 法测定川楝子中川楝素的研 究[J]. 西北药学杂志,2015,30(5):572 LÜ Z,ZHANG M,WANG L,et al. Determination of toosendanin in Toosendan Fructus by HPLC-MS/MS[J]. Northwest Pharm J, 2015,30(5):572
[13] 钟炽昌,谢晶曦,陈淑凤,等. 川楝素的化学结构[J]. 化学学报, 1975,33(1):35 ZHONG ZC,XIE JX,CHEN SF,et al. The chemical structure of toosendanin[J]. Acta Chim Sin,1975,33(1):35