摘要
目的建立同时测定小儿清降丸中绿原酸、连翘苷、丹皮酚、甘草酸铵、大黄素、大黄酚6种成分含量的高效液相色谱法。方法色谱柱为Agilent C18(4.6 mm×250 mm,5μm);流动相为乙腈(A)-0.1%磷酸水溶液(B),梯度洗脱条件:0~9 min,90%B;9~35 min,90%~50%B;35~50 min,50%~20%B,50~55 min,20%B;流速:1.0 ml·min^(-1);检测波长:240 nm;柱温:40℃;进样量:10μl。结果绿原酸、连翘苷、丹皮酚、甘草酸铵、大黄素和大黄酚分别在质量浓度为11.286~112.864μg·ml^(-1)(r=0.9998),0.902~9.025μg·ml^(-1)(r=0.9997),3.149~31.487μg·ml^(-1)(r=0.9998),0.396~3.955μg·ml^(-1)(r=0.9999),0.681~6.806μg·ml^(-1)(r=0.9998),3.106~31.063μg·ml^(-1)(r=0.9998)范围内与峰面积线性关系良好;精密度、稳定性、重复性试验结果的RSD均低于2.0%(n=6);平均加样回收率分别为98.97%,98.20%,99.13%,97.62%,98.01%,98.61%,RSD分别为1.47%,1.38%,1.15%,1.43%,1.88%,1.59%(n=6)。结论本研究所建立的测定方法专属性较强、重复性良好、测定结果准确,可用于同时测定小儿清降丸中6种有效成分的含量,为该医疗机构制剂品种的质量标准提升提供参考。
Objective To establish a high performance liquid chromatography method to determine the contents of six compounds Chlorogenic acid,Forsythin,Paeonol,Ammonium glycyrrhizate,Emodin and Chrysophanol in Xiaoer Qingjiang pills.Methods The HPLC gradient elution method was adopted on an Agilent C18 chromatographic column(4.6 mm×250 mm,5μm)with the mobile phase composed of acetonitrile(A)and-0.1%aqueous phosphoric acid solution(B)under gradient elution conditions(0-9 min,90%B;9-35 min,90%-50%B;35-50 min,50%-20%B;50-55 min,20%B)and at a flow rate of 1.0 ml·min^(-1).The detection wavelength was set at 240 nm.The column temperature was 40℃and the injection volume was 10μl.Results The linear ranges of Chlorogenic acid,Forsythin,Paeonol,Ammonium glycyrrhizate,Emodin and Chrysophanol were 11.286-112.864μg·ml^(-1)(r=0.9998),0.902-9.025μg·ml^(-1)(r=0.9997),3.149-31.487μg·ml^(-1)(r=0.9998),0.396-3.955μg·ml^(-1)(r=0.9999),0.681-6.806μg·ml^(-1)(r=0.9998),3.106-31.063μg·ml^(-1)(r=0.9998),respectively.The RSDs of test results of precision,stability and repeatability were lower than 2.0%(n=6).The average sample recovery of the added index was 98.97%,98.20%,99.13%,97.62%,98.01%,98.61%with RSDs of 1.47%,1.38%,1.15%,1.43%,1.88%and 1.59%(n=6),respectively.Conclusion This established determination method is exclusive,reproducible and accurate,which can be used to determine the contents of six active ingredients in Xiaoer Qingjiang pills simultaneously.This research can provide reference for improving the quality standard of this hospital-made preparation.
作者
马新玲
佟若菲
孙燕燕
MA Xin-ling;TONG Ruo-fei;SUN Yan-yan(Tianjin Children's Hospital(Children's Hospital,Tianjin University),Tianjin 300134,China)
出处
《解放军药学学报》
2023年第6期485-489,共5页
Pharmaceutical Journal of Chinese People's Liberation Army
基金
天津市医学重点学科(专科)建设项目,No.TJYXZDXK-040A。
关键词
医院制剂
高效液相色谱法
质量标准
含量测定
hospital-made preparation
high performance liquid chromatography
quality standard
content determination
