HPLC-DAD法同时测定小儿退热合剂中多指标成分含量

Simultaneous determination the contents of index components in Xiaoer Tuire mixture by HPLC-DAD

目的:建立同时测定小儿退热合剂中8个成分的方法。方法:采用DIKMA Platisil ODS色谱柱(250mm×4.6 mm,5μm),柱温35℃,流动相为乙腈-0.1%磷酸水溶液,采用梯度洗脱,变换波长检测,分别为240 nm(京尼平苷酸、京尼平龙胆双糖苷、京尼平苷)、274 nm(绿原酸、黄芩苷、丹皮酚)和210 nm(连翘苷、柴胡皂苷A),流速为1 mL·min^(-1)。结果:京尼平苷酸、京尼平龙胆双糖苷、京尼平苷、绿原酸、黄芩苷、丹皮酚、连翘苷、柴胡皂苷A的线性范围分别为1.17～9.36 ng·mL^(-1)(r=0.999 5),1.98～15.84 ng·mL^(-1)(r=0.999 7),8.00-64.00 ng·mL^(-1)(r=0.999 9),1.64～13.12 ng·mL^(-1)(r=0.999 8),7.00～56.00 ng·mL^(-1)(r=0.999 9),1.096～8.768 ng·mL^(-1)(r=0.999 9),0.56～4.48 ng·mL^(-1)(r=0.999 9),6.20～49.60 ng·mL^(-1)(r=0.999 8),平均回收率在95.2～103.0%之间。3批样品中上述8个成分的含量测定结果分别为0.124 4～0.125 2、0.172 4～0.172 9、1.331 4～1.331 9、0.129 2～0.130 3、1.543 3～1.544 1、0.107 3～0.107 6、0.304～0.308、0.373 0～0.374 5mg·mL^(-1)。结论:该法检测简便,稳定,可靠,可用于小儿退热合剂质量控制。

Objective:To establish a method for simultaneous determination of eight components in Xiaoer Tuire mixture.Methods:The separation was performed on a DIKMA Platisil ODS column(250 mm×4.6 mm,5 μm),column temperature was 35℃,acetonitriles and 0.1% H3PO4 aqueous solution was used as mobile phase for gradient elution.Detection wavelengths were 240 nm for geniposidic acid,genipin 1-gentiobioside,geniposide,274 nm for chlorogenic acid,baicalin,paeonol and 210 nm for phillyroside,saikosaponin A,respectively.The flow rate was 1 mL·min^-1.Results:Linear ranges of geniposidic acid,genipin 1-gentiobioside,geniposide,chlorogenic acid,baicalin,paeonol,phillyroside,saikosaponin A concentrations were 1.17-9.36 ng·mL^-1(r=0.999 5),1.98-15.84 ng·mL^-1(r=0.999 7),8.00-64.00 ng·mL^-1(r=0.999 9),1.64-13.12 ng·mL^-1(r=0.999 8),7.00-56.00 ng·mL^-1(r=0.999 9),1.096-8.768 ng·mL^-1(r=0.999 9),0.56-4.48 ng·mL^-1(r=0.999 9),6.20-49.60 ng·mL^-1(r=0.999 8),respectively.Their average recovery rates fell between 95.21% and 103.02%.The contents of the eight components in 3 batches of samples were 0.124 4-0.125 2,0.172 4-0.172 9,1.331 4-1.331 9,0.1292-0.130 3,1.543 3-1.544 1,0.107 3-0.107 6,0.304-0.308,0.373 0-0.374 5 mg·mL^-1.Conclusion:The method established is simple,stable,reliable and can be used as an effective method for quality control of Xiaoer Tuire mixture.