固相萃取-超高效液相色谱-串联质谱测定凉茶中15种植物源性兴奋剂和外源性药物

Determination of 15 Kinds of Plants Originated Stimulants and Exogenous Medicines Using Solid Phase Extraction Combined with UPLC-MS/MS

建立了固相萃取富集净化,超高效液相色谱-串联三重四级杆质谱（UPLC-MS/MS）测定凉茶中5种植物源性兴奋剂和10种外源性消炎镇痛类药物的方法。样品经高速离心后用甲酸调节至p H 4.0,HLB固相萃取柱净化,BEH C18色谱柱分离,乙腈-0.1%甲酸梯度洗脱,串联质谱电喷雾正、负离子扫描,多反应监测（MRM）模式检测,外标法定量。结果表明,15种待测物在1.0~200μg/L范围内线性关系良好;方法检出限（S/N=3）为0.1~2.0μg/L;添加水平为2.0~100μg/L时,平均回收率为76.4%~107%,相对标准偏差（RSD,n=6）为2.8%~9.7%,日间精密度为2.7%~12.0%。本方法前处理过程简单,净化效果好,灵敏度高,适用于凉茶中植物源性兴奋剂和外源性西药的检测。

An effective method was developed for the simultaneous determination of 15 kinds of plants originated stimulants and exogenous medicines in herbal tea using solid phase extraction（ SPE） combined with ultrahigh performance liquid chromatography-tandem mass spectrometry（ UPLC-MS / MS）. After centrifugation in high speed,the samples were purified using HLB SPE column at p H 4.0（ adjusted by formic acid）. A total of 15 targets were separated on a BEH C_（18） column by gradient elution with acetonitrile-0. 1% formic acid as mobile phase,ionized with positive and negative electrospray ionization（ ESI ＋ /-）,detected under multiple reaction monitoring（ MRM） mode,and quantified with external standard method. The method was validated by evaluating the linearity,recoveries,and precision. Favorable linearity was acquired in the concentration range of 1.0-200 μg / L,and the limits of detection（ LODs） were ranged from 0.1 to 2.0 μg / L. At the spiked levels of 2. 0- 100 μg / L,the average recoveries presented 76. 4%- 107. 0%,with the relative standard deviation（ RSD,n = 6） of 2. 8% to 9. 7% and intra-day precision of 2. 7%- 12. 0%. The procedure was successfully applied to the determination of plants originated stimulants and external medicines in commercial herbal tea.