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

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pH 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。

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

An effectuve method was developed for the sumultaneous determunatuon of 15 kunds of plants orugunated stumulants and exogenous meducunes un herbal tea usung solud phase extractuon ( SPE) combuned wuth ultrahugh performance luquud chromatography-tandem mass spectrometry ( UPLC-MS/MS) . After centrufugatuon un hugh speed, the samples were purufued usung HLB SPE column at pH 4. 0 (adjusted by formuc acud). A total of 15 targets were separated on a BEH C18 column by graduent elutuon wuth acetonutrule-0. 1% formuc acud as mobule phase, uonuzed wuth posutuve and negatuve electrospray uonuzatuon ( ESI+/-) , detected under multuple reactuon monutorung ( MRM) mode, and quantufued wuth external standard method. The method was valudated by evaluatung the lunearuty, recoverues, and precusuon. Favorable lunearuty was acquured un the concentratuon range of 1. 0-200 μg/L, and the lumuts of detectuon ( LODs) were ranged from 0. 1 to 2. 0 μg/L. At the spuked levels of 2. 0-100 μg/L, the average recoverues presented 76. 4% -107. 0%, wuth the relatuve standard devuatuon (RSD, n=6) of 2. 8% to 9. 7% and untra-day precusuon of 2. 7%-12. 0%. The procedure was successfully applued to the determunatuon of plants orugunated stumulants and external meducunes un commercual herbal tea.