银翘解毒制剂中咖啡因的筛查

Screening of Caffeine in Yinqiao Jiedu Preparations

目的采用LC-MS/MS法建立银翘解毒颗粒和银翘解毒丸中咖啡因的筛查方法。方法选择Agilent Poroshell 120 EC-C18柱(2.1 mm×100 mm,2.7μm),流动相为0.1%甲酸溶液-甲醇,采用梯度洗脱,流速为0.2 mL/min,柱温30℃,进样量5μL;采用ESI源负离子检测,MRM模式扫描,选择m/z 194.9→137.8和m/z 194.9→110.0作为检查离子对。结果咖啡因的进样浓度在22.173~1108.664 ng/mL呈良好线性关系(r=0.9974);咖啡因的平均回收率为100.7%,RSD为1.67%(n=6);6批次银翘解毒颗粒中检出咖啡因成分,含量范围为2.48~50.03μg/g。结论经方法学验证,该方法可用于银翘解毒颗粒和银翘解毒丸中咖啡因的筛查。

Objective To establish a LC-MS/MS method for screening caffeine in yinqiao jiedu granules and yinqiao jiedu pills.Methods Agilent Poroshell 120 EC-C18 column(2.1 mm×100 mm,2.7μm)was used.The mobile phase was 0.1%formic acid solution-methanol,using gradient elution,the detection flow rate was 0.2 mL/min,and the column temperature was maintained at 30°C,with an injection volume of 5μL.ESI source was used for negative ion detection,and MRM mode was used for scanning.The m/z 194.9→137.8 and m/z 194.9→110.0 were selected as the monitoring ions.Results The injection concentration of caffeine showed a good linear relationship between 22.173~1108.664 ng/mL(r=0.9974).The average recovery of caffeine was 100.7%with RSD of 1.67%(n=6).Caffeine was detected in 6 batches of yinqiao jiedu granules,and the content ranged from 2.48 to 50.03μg/g.Conclusion Methodological validation indicates that the established approach is suitable for screening caffeine in yinqiao jiedu granules and yinqiao jiedu pills.