文献类型：期刊文献

中文题名：UPLC-MS/MS同法测定熥敷颈腰痛酊中9个有效成分的含量

英文题名：Simultaneous determination of 9 active ingredients in Tongfu Jingyaotong tincture by UPLC-MS/MS

作者：赵继荣[1];杨文通[1];李硕[1];朱宝[2];李喜香[2];冯文渊[1];裴亮[1]

第一作者：赵继荣

机构：[1]甘肃中医药大学,兰州730030;[2]甘肃省中医院,兰州730050

第一机构：甘肃中医药大学

年份：2024

卷号：44

期号：6

起止页码：952

中文期刊名：药物分析杂志

外文期刊名：Chinese Journal of Pharmaceutical Analysis

收录：CSTPCD;;北大核心:【北大核心2023】；CSCD:【CSCD2023_2024】；

基金：甘肃省中医药项目(GZKZ-2020-3);甘肃省中医药产业精准对接就业创业人才科学化基地(3016170106)。

语种：中文

中文关键词：熥敷颈腰痛酊;超高效液相色谱串联质谱法;液质联用;活性成分;含量测定;质量控制

外文关键词：Tongfu Jingyaotong tincture;ultra-high performance liquid chromatography tandem mass spectrometry;LC-MS;active ingredients;Content determination;quality control

摘要：目的:建立一种同时测定熥敷颈腰痛酊中大豆苷元、芒柄花黄素、芫花素、槲皮素、芦丁、芹菜素、山柰酚、木犀草素、葛根素含量的超高效液相色谱串联质谱法(UPLC-MS/MS)。方法:采用Waters ACQUITY UPLC HSS T3色谱柱(100 mm×2.1 mm, 1.8μm),以0.1%甲酸水溶液为流动相A,甲醇为流动相B,梯度洗脱,流速为0.3 mL·min^(-1),柱温为45℃,进样量为2.0μL;电喷雾(ESI)离子源,正、负离子模式多反应监测采集。结果:芹菜素、芫花素、大豆苷元在0.2~1 000 ng·mL^(-1)范围内线性良好,葛根素、芦丁、木犀草素、山柰酚、芒柄花黄素在0.2~2 000 ng·mL^(-1)范围内线性良好,槲皮素在1.0~5 000 ng·mL^(-1)范围内线性良好;分离度较好,精密度、重复性、重现性、稳定性试验RSD均小于5%(n=6);平均加样回收率在82.7%~111.8%,RSD为2.0%~5.4%(n=6)。6批熥敷颈腰痛酊中大豆苷元、芒柄花黄素、芫花素、槲皮素、芦丁、芹菜素、山柰酚、木犀草素、葛根素的含量范围分别为8.46~17.97μg·mL^(-1)、0.62~1.67μg·mL^(-1)、0.03~0.08μg·mL^(-1)、1.34~2.22μg·mL^(-1)、0.70~1.14μg·mL^(-1)、0.48~0.99μg·mL^(-1)、0.20~0.90μg·mL^(-1)、0.10~0.16μg·mL^(-1)、167.95~227.75μg·mL^(-1)。结论:本方法专属性强,线性范围宽,准确高效,可同时对熥敷颈腰痛酊中9个有效成分进行含量检测,为该方建立有效的质量控制方法。
Objective:To establish an ultra-high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)for the simultaneous determination of daidzein,formononetin,genkwanin,quercetin,rutin,apigenin,kaempferol,luteolin and puerarin in Tongfu Jingyaotong tincture.Methods:The Waters ACQUITY UPLC HSS T3 Column(100 mm×2.1 mm,1.8μm)was used with methanol and 0.1%formic acid(gradient elution)as the mobile phase at a flow rate of 0.3 mL·min^(-1).Column temperature was 45℃,and injection volume was 2.0μL.Electrospray ion source was adopted with positive and negative ion modes and multi-reaction monitoring and acquisition.Results:Apigenin,genkwanin and daidzein had good linearity in the range of 0.2-1000 ng·mL^(-1),puerarin,rutin,luteolin,kaempferol and formononetin in the range of 0.2-2000 ng·mL^(-1),and quercetin in the range of 1.0-5000 ng·mL^(-1).The resolution was good,and the RSDs of precision,repeatability,reproducibility and stability test were all below 5%(n=6).The average recoveries ranged from 82.7%to 111.8%with RSDs(n=6)of 2.0%-5.4%.The contents of daidzein,formononetin,genkwanin,quercetin,rutin,apigenin,kaempferol,luteolin and puerarin in 6 batches of Tongfu Jingyaotong tincture were 8.46-17.97μg·mL^(-1),0.62-1.67μg·mL^(-1),0.03-0.08μg·mL^(-1),1.34-2.22μg·mL^(-1),0.70-1.14μg·mL^(-1),0.48-0.99μg·mL^(-1),0.20-0.90μg·mL^(-1),0.10-0.16μg·mL^(-1)and 167.95-227.75μg·mL^(-1),respectively.Conclusion:This method has strong specificity,wide linear range,accuracy and efficiency,and can detect the contents of 9 active ingredients in Tongfu Jingyaotong tincture at the same time,which offers an effective quality control method for Tongfu Jingyaotong tincture.