UHPLC-MS/MS法同时测定苏桔口服液中4种成分的含量

Simultaneous determination of four components in Sujie Oral Liquid by UHPLC-MS/MS

目的建立超高效液相色谱-三重四级杆串联质谱(UHPLC-MS/MS)同时快速测定苏桔口服液中甘草苷、迷迭香酸、桔梗皂苷D、甘草酸4种成分质量浓度的分析方法,以期更全面控制苏桔口服液的质量。方法样品采用Agilent Extend C18(2.1 mm×100 mm,1.7μm)色谱柱分离,柱温为35℃,以0.1%甲酸水(A)-乙腈(B)为流动相进行梯度洗脱,流速为0.3 mL/min;质谱采用电喷雾离子源,多重反应监测模式下负离子同时测定,检测离子对为甘草苷417.1/255.1(135)、迷迭香酸359.0/197.1(160.9)、桔梗皂苷D 1223.6/681.0、甘草酸821.4/350.9。结果4种成分在一定质量浓度范围内呈良好线性关系(r>0.999),平均加样回收率为98.80%~100.84%,RSD为1.82%~2.53%;10批苏桔口服液样品中,甘草苷、迷迭香酸、桔梗皂苷D、甘草酸的质量浓度分别为0.1408~0.1592、0.0824~0.1421、0.0359~0.0698、0.6659~0.7238 mg/mL。结论建立的多成分质量浓度检测方法快速、准确、重现性高,可为有效评价苏桔口服液的质量提供依据。

Objective To establish a method for the simultaneous and rapid determination of four components,i.e.liquiritin,rosmarinic acid,platycodon D and glycyrrhizic acid in Sujie Oral Liquid by ultra high performance liquid chromatography-tandem quadrupole mass spectrometry(UHPLC-MS/MS),so as to control the quality of Sujie Oral Liquid.Methods The samples were separated on an Agilent Extend C18(2.1 mm×100 mm,1.7μm)column with a mobile phase containing 0.1%formic acid(A)and acetonitrile(B)by gradient elution.The column temperature was set at 35℃,and the flow rate was 0.3 mL/min.ESI ion source was used.In multiple reaction monitoring mode,they were analyzed in negative ion mode.The ion pairs were as follows:liquiritin 417.1/255.1(135),rosmarinic acid 359/197.1(160.9),platycodon D 1223.6/681.0,glycyrrhizic acid 821.4/350.9.Results The four components showed good linear relationships within their mass concentration ranges(r>0.999),whose average recoveries were 98.80%-100.84%with the RSDs of 1.82%-2.53%.In 10 batches of Sujie Oral Liquids,the mass concentrations of liquiritin,rosmarinic acid,platycodon D,and glycyrrhizic acid were 0.1408-0.1592,0.0824-0.1421,0.0359-0.0698,and 0.6659-0.7238 mg/mL,respectively.Conclusion The method of simultaneous determination for four components in Sujie Oral Liquid is fast,accurate and highly reproducible,which provides experimental basis for the quality evaluation of Sujie Oral Liquid.