QuEChERS前处理结合HPLC-Q-TOF/MS非靶向快速筛查凉茶中的非法添加物

建立了QuEChERS法净化,结合高效液相色谱-四极杆-飞行时间质谱法(HPLC-Q-TOF/MS)非靶向快速筛查凉茶中未知非法添加物的方法。凉茶中的非法添加物经0.5%乙酸-乙腈提取,氨丙基粉净化,C₁₈色谱柱(100 mm×2.1 mm,1.7μm)分离,HPLC-Q-TOF/MS测定。利用8种质控化合物建立的筛查方法检出限为2.0～10μg/kg,定量下限为5.0～25μg/kg。3个不同加标水平的平均回收率为75.8%～95.6%,RSD(n=6)为2.1%～6.5%。在该定量方法基础上利用目标化合物特征离子的精确质量数、同位素匹配、二级碎片信息进行数据库匹配,无标准品情况下非靶向筛查非法添加物。结果表明,该方法无需标准品即可快速筛查凉茶中的非法添加西药,能应用于凉茶样品的实际筛查。应用该方法对50份散装凉茶样品进行测定,其中10份凉茶样品检出对乙酰氨基酚,含量为4.14～2 188 mg/kg。该方法快速、准确、分析通量高,可为凉茶中非法添加物的快速筛查和质量控制提供重要依据。

Non-target Screening of Illegal Additive Residues in Herbal Teas by High Performance Liquid Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry with QuEChERS Purification

A high performance liquid chromatography-quadrupole-time-of-flight mass spectrometric (HPLC-Q-TOF/MS )method with a modified QuEChERS purification was developed for the rapid screening of unkown illegal additive residues in herbal teas.The target compounds in samples were extracted with 0.5 % acetic acid-acetonitrile,cleaned with NH 2 sorbent and separated on a C 18 column (100 mm×2.1 mm,1.7 μm ),then determined by HPLC-Q-TOF/MS.The detection limits and the quantitation limits for 8 control drugs were in the ranges of 2.0-10 μg/kg and 5.0-25 μg/kg,respectively.The average recoveries for the samples at three spiked levels ranged from 75.8 % to 95.6 %,with RSD ( n= 6 )of 2.1 %-6.5 %.Moreover,the acquired data were compared with the library using the accurate mass,isotopic distribution,fragmentation information to screen illegal additive residues in herbal teas without reference standards.The developed method was used in the determination of 50 herbal tea samples.Results showed that paracetamol was detected in 10 samples,with content range of 4.14-2 188 mg/kg.This method is efficient,sensititive and accurate,and could meet the requirement for rapid screening of unkown illegal additive residues in herbal teas.