QuEChERS-UPLC-MS/MS测定火锅汤料中6种非法添加化学药物

建立采用分散固相萃取前处理结合超高效液相色谱-串联质谱法同时测定火锅汤料中6 种解热镇痛类药物(对乙酰氨基酚、氯苯那敏、双氯芬酸钠、阿司匹林、氨基比林、安替比林)的方法。结果表明,样品经0.1%甲酸-乙腈提取,无水硫酸镁和乙酸钠盐析脱水,离心后上层有机相用100 mg乙二胺-N-丙基硅烷(primarysecondary amine,PSA)、100 mg十八烷基硅烷(C18)和50 mg石墨化碳黑(Graphitized carbon blacks,GCB)萃取净化,采用Waters C₁₈色谱柱(50 mm×2.1 mm,1.7 μm)分离,用乙腈和0.1%甲酸水溶液作为流动相梯度洗脱分离,采用电喷雾-正/负离子多反应监测模式检测,外标法定量。在1.0~200 ng/mL(阿司匹林10.0~2000 ng/mL)的质量浓度范围内,6种化学药物的线性决定系数均大于0.99,该方法的检出限在0.05~1.0 μg/kg之间。在火锅汤料进行3 个水平添加实验(n=6),6种化学药物的回收率为72.1%~114.8%,相对标准偏差为0.81%~14.6%。本方法简单快速、准确度好、精密度高,适合于火锅汤料中6 种非法添加化学药物残留量的同时检测。

Determination of Six Chemicals Illegally Added in Hot Pot Soup by QuEChERS Combined with UPLC-MS/MS

A method for the determination of six analgesic-antipyretic drugs (paracetamol, chlorpheniramine maleate, diclofenac sodium, aspirin, aminophenazone and antipyrine) illegally added in hot pot soup by QuEChERS combined ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. The hot pot soup samples were extracted with 0.1% formic acid in acetonitrile followed by a salting-out step with anhydrous MgSO₄ and CH₃COONa. After centrifugation, the supernatant was cleaned up with 100 mg of PSA, 100 mg of C₁₈ and 50 mg of GCB. The separation was performed on a Waters C₁₈ column (50 mm×2.1 mm, 1.7 μm) by gradient elution acetonitrile with and water containing 0.1% formic acid. The electrospray ionization mass spectrometry was operated in the positive and negative mode using multiple reaction monitoring (MRM). The target compounds were quantified by external standard method. Under the optimal conditions, the calibration curves of the six chemicals were linear in the concentration range of 1.0~200 ng/mL (aspirin 10.0~2000 ng/mL) with correlation coefficients larger than 0.99. The limits of detection (LOD) ranged from 0.05~1.0 μg/kg. The average recoveries for hot pot soup at three spiked levels ranged from 72.1%~114.8% with relative standard deviations (RSDs) of 0.81%~14.6%. The method was suitable for the simultaneous detection of 6 illegally added chemicals in hot pot soup with its rapidity, high accuracy and high precision.