QuEChERS-液质联用法快速测定凉茶中非法添加的10种止咳平喘类化学药物

建立凉茶中地塞米松、氨溴索、布地奈德等10种非法添加的止咳平喘类化学药物的QuEChERS结合高效液相色谱-串联质谱的检测方法。样品经乙腈提取,应用QuEChERS技术净化,经0.22 μm微孔滤膜过滤,以乙腈-10 mmol/L醋酸铵溶液(含0.1%甲酸)为流动相梯度洗脱,并在Agilent SB-C18柱(100 mm×4.6 mm,2.7 μm)上实现10种化学药物的基线分离。该方法采用多反应监测(MRM)正离子模式扫描,标准曲线外标法定量。10种待测物在各自的浓度范围内,线性关系良好,相关系数均不小于0.9984,检出限为0.1~3.0 μg/L。在三个不同添加水平下的平均回收率为67.1%~108.5%,相对标准偏差(RSD)为0.2%~6.9%。该方法操作简单,净化效果好,灵敏度高,可用于凉茶中10种非法添加的止咳平喘类化学药物的快速分析。

Rapid Determination of Ten Chemical Drugs for the Treatment of Cough and Asthma added Illegally in Herbal Tea by HPLC -MS/MS Coupled with Modified QuEChERS

A high performance liquid chromatography-tandem mass spectrometric method with modified QuEChERS method for sample preparation was developed for the simultaneous determination of 10 chemical drugs added illegally in herbal tea. The samples were extracted with acetonitrile,purified with QuEChERS method and filtrated by 0.22 μm microporous filters. The separation was carried on an Agilent SB-C18 Column(100 mm×4.6 mm,2.7 μm)by a gradient elution using acetonitrile-0.01 mol/L ammonium acetate solution(contain 0.1% formic acid aqueous)as mobile phase. The analytes were detected by tandem mass spectrometry under multiple reaction monitoring(MRM)mode with positive electrospray ionization(ESI+)and quantified by external standard calibration method. The correlation coefficients of the standard calibration curves for the 10 analytes were all above 0.9984.The limits of detection was 0.1~3.0 μg/L. The blank samples were fortified at three levels,and the average recoveries ranged from 67.1% to 108.5% with the RSDs from 0.2% to 6.9%. The method developed was easy to operate,sensitive,and had good purification effect. It could be applied for the rapid determination of ten chemical drugs added illegally for the treatment of cough and asthma in herbal tea.