论文部分内容阅读
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。
Shegan Mixture and Gandhi Capsule are two traditional Chinese medicine compound preparations in Xinhua Hospital. The UHPLCMS / MS method was established for the simultaneous determination of ephedrine, caffeic acid, ferulic acid, rutin, wild baicalin, , Baicalin, baicalein, Astragaloside IV, the second wild tectorigenin, wogonin and other 11 kinds of Chinese medicine ingredients. The column was eluted with ZORBAX SBC18 (2.1 mm × 50 mm, 1.8 μm) and the mobile phase consisted of 0.1% formic acid in acetonitrile with a flow rate of 0.3 mL / min and a column temperature of 35 o C. The electrospray ionization (ESI ), Multi-reactive ion monitoring (MRM), combined with positive and negative ion scanning switch, in which caffeic acid, ferulic acid, wild baicalin, dry glycosides detected by negative mode, ephedrine, rutin, baicalin, baicalein, Astragalus A Glycosides, the second wild Iris flavin, wogonin using positive ion mode detection. The results showed that the limit of quantification of ephedrine, caffeic acid, ferulic acid, rutin, wild baicalin, cantharidin, baicalin, baicalein, Astragaloside IV, the second wild tectorigenin, wogonin were 4.90 × 10- 3 ng / mL, 7.80 ng / mL, 6.8 ng / mL, 5.3x10-2 ng / mL, 4.20x10-3 ng / mL, 4.6x10-2 ng / mL, 1.44x10-4 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 were 2.90 × 10-4 ng / mL, 0.77 ng / mL and 2.0 ng / mL, 0.016 ng / mL, 1.3x10-3 ng / mL, 3.33x10-4 ng / mL, 4.32x10-5 ng / mL, 1.46 ng / mL, 0.07 ng / mL, 9.5x10-5 ng / mL, 8.84 × 10-5 ng / mL. R 2> 0.99 over the corresponding linear range. Both intra- and inter-day precision (RSD) were less than 5% with an average recovery of 80% -120%. The method can realize the separation and determination of 11 target compounds within 20 min, and is simple, rapid, sensitive and accurate, and can be used for determining the content of indicator components of Shegan Mixture and Gandi Capsule, thereby providing the basis for quality control of the two preparations.