摘要
目的：建立一种高效液相色谱质谱联用法同时测定黄芩苷、野黄芩苷、汉黄芩素、咖啡酸、麻黄碱、射干苷、次野鸢尾黄素、黄芩素等8种中药成分的含量及其在我院自有制剂射干合剂中的应用。方法：色谱条件：色谱柱为ZORBAX SB-C18（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^-1,柱温：35℃;质谱条件：采用电喷雾离子源（ESI）,多反应离子监测（MRM）,结合正负离子扫描切换,其中咖啡酸、野黄芩苷、射干苷采用负离子模式检测,黄芩苷、汉黄芩素、次野鸢尾黄素、黄芩素、麻黄碱采用正离子模式检测。结果：黄芩苷、野黄芩苷、汉黄芩素、咖啡酸、麻黄碱、射干苷、次野鸢尾黄素、黄芩素的定量限分别为1.44×10^-4,4.20×10^-3,2.95×10^-4,7.80,4.90×10^-3,4.6×10-2,3.18×10^-4,4.85 ng·mL^-1,检测限分别为4.32×10^-5,1.3×10^-3,8.84×10^-5,0.77,2.90×10^-4,3.33×10^-4,9.5×10^-5,1.46 ng·mL^-1;在相应的线性范围内R^2〉0.992 3;日内和日间精密度（RSD）均小于5%,平均回收率均在80%-120%。结论：本方法在20 min内实现这8种化合物的分离和测定,简单、快速、灵敏、准确,可用于射干合剂多成分含量测定。
Objective： To establish an UHPLC-MS / MS method to determine the contents of baicalin,scutellarin,wogonin,caffeic acid,ephedrine,belamcandin,irisflorentin and baicalein in Shegan mixtures. Methods： The chromatographic separation was performed on a ZORBAX SB-C18column（ 2. 1 mm × 50 mm,1. 8 μm） with the mobile phase consisting of acetonitrile and water（ 0. 1% formic acid）,the flow rate was 0. 3 ml·min^-1,and the column temperature was 35℃. Electrospray ionization source（ ESI） was used with multiple reaction monitoring（ MRM） combined with positive and negative scanning switch. Negative ion mode detection was used for caffeic acid,belamcandin and scutellarin,while positive ion mode detection was used for baicalin,wogonin,irisflorentin,baicalein and ephedrine. Results： The quantification limit of baicalin,scutellarin,wogonin,caffeic acid,ephedrine,belamcandin,irisflorentin and baicalein was 1. 44 × 10^-4,4. 20 ×10^-3,2. 95 ×10^-4,7. 80,4. 90 ×10^-3,4. 6 ×10- 2,3. 18 ×10^-4ng·mL^-1and 4. 85 ng·mL^-1. The detection limit was 4. 32 × 10^-5,1. 3 × 10^-3,8. 84 × 10^-5,0. 77,2. 90 × 10^-4,3. 33 × 10^-4,9. 5 × 10^-5ng ·mL^-1and 1. 46 ng ·mL^-1,respectively. The correlation coefficients（ R^2） were all higher than 0. 992 3 within the linear ranges. Both intra- and inter-day RSD were less than 5%. The average recoveries of the eight components were within the range of 80%-120%. Conclusion： The method is simple,rapid,sensitive and accurate. It can be used to determine the contents of baicalin,scutellarin,wogonin,caffeic acid,ephedrine,belamcandin,irisflorentin and baicalein in Shegan mixtures for the quality control.
出处
《中国药师》
CAS
2015年第4期574-578,共5页
China Pharmacist
基金
上海市卫生局中医药科研基金(编号:2012G003A)
上海市教委优秀青年教师基金(编号:ZZjdyx13092)
关键词
液相色谱-质谱联用
射干合剂
含量测定
Liquid chromatography-mass spectrometry
Shegan mixtures
Content determination
