摘要
In the present study, we established an ultra-high pressure liquid chromatography-tandem mass spectrometry （UHPLC-MS/MS） method to simultaneously determine 11 compounds in two hospital preparations （Shegan mixture and Gandi capsules）, including ephedrine, caffeic acid, ferulic acid, rutin, scutellarin, belamcandin, baicalin, baicalein, astragaloside IV, irisflorentin and wogonin. The chromatographic separation was conducted on ZORBAX SB-C18 （2.1 mm×50 mm, 1.8 μm）. Eleven analytes and IS were detected using ESI and MRM combined with positive and negative scanning switch. Caffeic acid, ferulic acid, scutellarin and belamcandin were detected using negative ion mode detection, whereas ephedrine, rutin, baicalin, baicalein, astragaloside IV, irisflorentin and wogonin were detected using positive ion mode detection. The quantification limits of ephedrine, caffeic acid, scutellarin, belamcandin, baicalin, baicalein, irisfiorentin and wogonin were 4.90×10^-3 ng/mL, 7.80 ng/mL, 6.8 ng/mL, 5.3×10^-2 ng/mL, 4.20×10^-3 ng/mL, 4.6×10^-2 ng/mL, 1.44×10^-4 ng/mL, 4.85 ng/mL, 0.23 ng/mL, 3.18× 10^-4 ng/mL and 2.95× 10^-4 ng/mL, respectively. The detection limits of these components were 2.90× 10^-4 ng/mL, 0.77 ng/mL, 2.0 ng/mL, 0.016 ng/mL, 1.3×10^-3 ng/mL, 3.33×10^-4 ng/mL, 4.32×10^-5 ng/mL, 1.46 ng/mL, 0.07 ng/mL, 9.5×10^-5 ng/mL and 8.84× 10^-5 ng/mL, respectively. All calibration curves showed good linearity （R^2〉0.99） within the test range. The RSD values of intra-day and inter-day precision were less than 5%, and the average recovery rates of the 11 components ranged fi＇om 80% to 120%. In conclusion, our newly developed method was simple, rapid, sensitive and accurate. It could be used to determine ephedrine, caffeic acid, ferulic acid, rutin, scutellarin, belamcandin, baicalin, baicalein, astragaloside IV, irisflorentin and wogonin in Shegan mixture and Gandi capsules, which was helpful for the quality control of drugs.
射干合剂和甘地胶囊是新华医院的两个院内中药复方制剂,本文建立了UHPLCMS/MS方法同时测定这两个制剂中的麻黄碱、咖啡酸、阿魏酸、芦丁、野黄芩苷、射干苷、黄芩苷、黄芩素、黄芪甲苷、次野鸢尾黄素、汉黄芩素等11种中药成分的含量。色谱柱采用ZORBAX SBC18(2.1 mm×50 mm,1.8μm),流动相为0.1%甲酸水溶液–乙腈,梯度洗脱,流速为0.3 mL/min,柱温35 oC.质谱采用电喷雾离子源(ESI),多反应离子监测(MRM),并结合正负离子扫描切换,其中咖啡酸、阿魏酸、野黄芩苷、射干苷采用负离子模式检测,麻黄碱、芦丁、黄芩苷、黄芩素、黄芪甲苷、次野鸢尾黄素、汉黄芩素采用正离子模式检测。结果显示麻黄碱、咖啡酸、阿魏酸、芦丁、野黄芩苷、射干苷、黄芩苷、黄芩素、黄芪甲苷、次野鸢尾黄素、汉黄芩素的定量限分别为4.90×10–3 ng/mL、7.80 ng/mL、6.8 ng/mL、5.3×10–2 ng/mL、4.20×10–3 ng/mL、4.6×10–2 ng/mL、1.44×10–4 ng/mL、4.85 ng/mL、0.23 ng/mL、3.18×10–4 ng/mL、2.95×10–4 ng/mL,检测限分别为2.90×10–4 ng/mL、0.77 ng/mL、2.0 ng/mL、0.016 ng/mL、1.3×10–3 ng/mL、3.33×10–4 ng/mL、4.32×10–5 ng/mL、1.46 ng/mL、0.07 ng/mL、9.5×10–5 ng/mL、8.84×10–5 ng/mL。在相应的线性范围内R 2>0.99.日内和日间精密度(RSD)均小于5%,平均回收率均在80%–120%。本方法在20 min内实现这11种目标化合物的分离和测定,简单、快速、灵敏、准确,可用于射干合剂和甘地胶囊的指标成分含量测定,为这两个制剂的质量控制提供依据。
基金
Shanghai Science and Technology Commission Research Fund(Grant No.11DZ1972500)
Shanghai Health Bureau of Traditional Chinese Medicine Research Fund(Grant No.2012G003A)
Shanghai Municipal Education Commission of Outstanding Young Teachers in Special Fund(Grant No.ZZjdyx13092)
