CAJ | 학술논문

建立了凉茶中马来酸氯苯那敏、吡罗昔康、α-细辛脑等12种非法添加的化学药物的 QuEChERS 结合超高效液相色谱-串联质谱（ UPLC-MS／MS）的检测方法。样品经乙腈提取，应用 QuEChERS 技术净化，经0.22μm 微孔滤膜过滤后进行 UPLC-MS／MS 测定，以乙腈-0.1％（ v／v）乙酸水溶液为流动相梯度洗脱，在 XBridge BEH C18柱（100 mm×2.1 mm，3.5μm）上实现12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。12种待测物在各自的质量浓度范围内线性关系良好，相关系数均大于0.997，检出限为0.1~2.1μg／L，定量限为0.4~8.0μg／L。在3个不同添加水平下的平均回收率为62.7％~95.2％，RSD为1.3％~10.8％。应用该方法对市面上销售的74批次凉茶进行了筛查测定，部分样品的测定结果为阳性。该方法操作简单，净化效果好，灵敏度高，适用于凉茶中12种非法添加的化学药物的快速分析。
건립료량다중마래산록분나민、필라석강、α-세신뇌등12충비법첨가적화학약물적 QuEChERS 결합초고효액상색보-천련질보（ UPLC-MS／MS）적검측방법。양품경을정제취，응용 QuEChERS 기술정화，경0.22μm 미공려막과려후진행 UPLC-MS／MS 측정，이을정-0.1％（ v／v）을산수용액위류동상제도세탈，재 XBridge BEH C18주（100 mm×2.1 mm，3.5μm）상실현12충화학약물적기선분리。해방법채용다반응감측（MRM）정리자모식소묘，표준곡선외표법정량。12충대측물재각자적질량농도범위내선성관계량호，상관계수균대우0.997，검출한위0.1~2.1μg／L，정량한위0.4~8.0μg／L。재3개불동첨가수평하적평균회수솔위62.7％~95.2％，RSD위1.3％~10.8％。응용해방법대시면상소수적74비차량다진행료사사측정，부분양품적측정결과위양성。해방법조작간단，정화효과호，령민도고，괄용우량다중12충비법첨가적화학약물적쾌속분석。
An ultra high performance liquid chromatography-tandem mass spectrometry method with modified QuEChERS procedure for sample preparation was developed for the simultaneous determination of 12 chemical drugs(chlorpheniramine,piroxicam,α-asarone etc)illegally added in herbal tea. The samples were extracted with acetonitrile,purified with QuEChERS procedure and filtrated by 0. 22 μm microporous filters. The separation was carried on an XBridge BEH C18 column(100 mm×2. 1 mm,3. 5 μm)by a gradient elution using acetonitrile/0. 1%( v/v)formic acid aqueous solution as mobile phases. The analytes were detected by tan-dem mass spectrometry with positive electrospray ionization( ESI+)in multiple reaction moni-toring( MRM)mode,and quantified by external standard calibration method. The correlation coefficients of the standard calibration curves for the 12 analytes were all above 0. 997. The lim-its of detection ranged from 0. 1 μg/L to 2. 1 μg/L,and the limits of quantification ranged from 0. 4 μg/L to 8. 0 μg/L. The average recoveries of the 12 analytes spiked at three levels in blank samples ranged from 62. 7% to 95. 2% with the RSDs from 1. 3% to 10. 8%. The samples bought from markets were screened,and some of the samples showed positive for these analytes. The method developed is easy to operate,sensitive,and with good purification effect. It can be applied to the rapid determination of the 12 chemical drugs illegally added in herbal tea.