摘要
目的:建立LC-MS/MS法同时测定小儿豉翘清热颗粒中栀子苷、芍药内酯苷、芍药苷、连翘酯苷A、甘草苷、黄芩苷、连翘苷、千层纸素A-7-O-β-D-葡萄糖醛酸苷、汉黄芩苷、黄芩素、汉黄芩素、大黄酸、甘草酸共13个成分的含量。方法:采用Poroshell 120 SB-C;色谱柱(100 mm×3.0 mm,2.7μm),以0.1%甲酸水与甲醇-乙腈(1∶1)为流动相,梯度洗脱,流速0.45 mL·min^(-1),柱温40℃;采用电喷雾(ESI)离子源,多反应监测模式(MRM)进行负离子扫描。结果:栀子苷质量浓度在9~900 ng·mL^(-1),芍药内酯苷在1~100 ng·mL^(-1),芍药苷在12~1200 ng·mL^(-1),连翘酯苷A在12~1800 ng·mL^(-1),甘草苷在1~100 ng·mL^(-1),黄芩苷在8~800 ng·mL^(-1),连翘苷在5~500 ng·mL^(-1),千层纸素A-7-O-β-D-葡萄糖醛酸苷在5~500 ng·mL^(-1),汉黄芩苷在5~500 ng·mL^(-1),黄芩素在2~200 ng·mL^(-1),汉黄芩素在0.4~40 ng·mL^(-1),大黄酸在0.4~40 ng·mL^(-1),甘草酸在5~500 ng·mL^(-1)范围内线性关系良好(r>0.9985);平均加样回收率(n=6)范围均为97.0%~110.5%,RSD为3.2%~9.6%;5个批次样品中,13个成分的含量分别为栀子苷4.933~5.800 mg·g^(-1),芍药内酯苷0.104~0.123 mg·g^(-1),芍药苷3.140~4.159 mg·g^(-1),连翘酯苷A 17.40~21.05 mg·g^(-1),甘草苷0.354~0.425 mg·g^(-1),黄芩苷4.991~6.422 mg·g^(-1),连翘苷1.446~1.906 mg·g^(-1),千层纸素A-7-O-β-D-葡萄糖醛酸苷0.441~0.534 mg·g^(-1),汉黄芩苷0.925~1.138 mg·g^(-1),黄芩素0.129~0.151 mg·g^(-1),汉黄芩素0.084~0.106 mg·g^(-1),大黄酸0.051~0.063 mg·g^(-1),甘草酸0.964~1.242 mg·g^(-1)。结论:该方法特异、灵敏、高效、可靠,可用于小儿豉翘清热颗粒的质量控制。
Objective:To establish an LC-MS/MS method for simultaneous determination of 13 components(geniposide,albiflorin,paeoniflorin,forsythoside A,liquiritin,baicalin,forsythin,oroxylin A-7-O-β-D-glucuronide,wogonoside,baicalein,wogonin,rhein and glycyrrhizic acid)in Xiao’er Chiqiao Qingre granules.Methods:The separation was performed on a Poroshell 120 SB-C;column(100 mm×3.0 mm,2.7μm)by gradient elution,with mobile phase consisting of 0.1%formic acid aqueous and methanol-acetonitrile(1∶1)at a flow rate of 0.45 mL·min^(-1)and the column temperature of 40℃.The MS analysis was performed on a triple quadrupole mass spectrometer with an electrospray ionization(ESI)source operated in negative ion mode and multiple reaction monitoring(MRM).Results:The method had a good linearity in the ranges of 9-900 ng·mL^(-1)for geniposide,1-100 ng·mL^(-1)for albiflorin,12-1200 ng·mL^(-1)for paeoniflorin,12-1800 ng·mL^(-1)for forsythoside A,1-100 ng·mL^(-1)for liquiritin,8-800 ng·mL^(-1)for baicalin,5-500 ng·mL^(-1)for forsythin,5-500 ng·mL^(-1)for oroxylin A-7-O-β-D-glucuronide,5-500 ng·mL^(-1)for wogonoside,2-200 ng·mL^(-1)for baicalein,0.4-40 ng·mL^(-1)for wogonin,0.4-40 ng·mL^(-1)for rhein and 5-500 ng·mL^(-1)for glycyrrhizic acid(r>0.9985).The average recoveries(n=6)of them were 97.0%-110.5%with the RSDs of 3.2%-9.6%.The contents of 13 components in 5 batches of Xiao’er Chiqiao Qingre granules were 4.933-5.800 mg·g^(-1)of geniposide,0.104-0.123 mg·g^(-1)of albiflorin,3.140-4.159 mg·g^(-1)of paeoniflorin,17.40-21.05 mg·g^(-1)of forsythoside A,0.354-0.425 mg·g^(-1)of liquiritin,4.991-6.422 mg·g^(-1)of baicalin,1.446-1.906 mg·g^(-1)of forsythin,0.441-0.534 mg·g^(-1)of oroxylin A-7-O-β-D-glucuronide,0.925-1.138 mg·g^(-1)of wogonoside,0.129-0.151 mg·g^(-1)of baicalein,0.084-0.106 mg·g^(-1)of wogonin,0.051-0.063 mg·g^(-1)of rhein and 0.964-1.242 mg·g^(-1)of glycyrrhizic acid.Conclusion:The method is specific,sensitive,effective and reliable,and can be used for quality control of Xiao’er Chiqiao Qing
作者
李超
赵权
田刚
朱法根
吴菲
居文政
欧阳冰琛
LI Chao;ZHAO Quan;TIAN Gang;ZHU Fa-gen;WU Fei;JU Wen-zheng;OUYANG Bing-chen(Jumpcan Pharmaceutical Co.,Ltd.,Taizhou 225411,China;Department of Clinical Pharmacology,Affiliated Hospital of Nanjing University of Chinese Medicine,Nanjing 210029,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2022年第4期572-579,共8页
Chinese Journal of Pharmaceutical Analysis
基金
国家医药管理局标准化建设项目(ZYBZH-C-JS-33)。
