超高效液相色谱三重四极杆复合线性离子阱质谱法测定预制菜中15种非法添加化学药物

Determination of 15 kinds of chemicals illegally added in prefabricated food by ultra performance liquid chromatography-triple quadrupole composite linear ion trap mass spectrometry

中文关键词:  非法添加物  预制菜  通过型固相萃取  线性离子阱质谱法  多反应监测触发增强子离子扫描

英文关键词:illegal additives  prefabricated food  pass-through solid phase extraction  linear ion trap mass spectrometry  multiple reaction monitoring-information dependent acquisition-enhanced product ion

中文摘要:

      目的 建立超高效液相色谱三重四极杆复合线性离子阱质谱法的多反应监测-信息依赖性采集-增强子离子扫描(multiple reaction monitoring-information dependent acquisition-enhanced product ion, MRM-IDA-EPI)方式结合通过型固相萃取技术测定预制菜中15种非法添加化学药物的方法。方法 样品用1%(体积分数)甲酸乙腈提取, 通过型固相萃取柱Captiva EMR-Lipid净化, 以乙腈-0.05%(体积分数)甲酸水(含5 mmol/L乙酸铵)为流动相, Agilent Poroshell 120 EC-C18 (2.1 mm×100 mm, 1.9 μm)色谱柱进行分离, 采用MRM-IDA-EPI的扫描方式, 外标法定量。结果 15种目标物在一定范围内, 线性相关系数范围为0.9956~0.9996。该方法的检出限在0.62~62.50 μg/kg。预制菜进行3个水平添加实验(n=6), 15种目标物的平均回收率为78.33%~109.51%, 精密度为0.67%~14.02%。结论 该方法简单快速, 准确度好, 精密度高, 适用于预制菜中非法添加15种化学药物的检测, 可为预制菜的质量检测及市场监管提供技术支撑。

英文摘要:

      Objective To establish a method for the determination of 15 kinds of chemicals illegally added in prefabricated food by ultra performance liquid chromatography-triple quadrupole composite linear ion trap mass spectrometry in multiple reaction monitoring-information dependent acquisition-enhanced product ion (MRM-IDA-EPI) mode combined with pass-through solid phase extraction technology. Methods The samples were extracted with 1% (volume fraction) formic acid in acetonitrile. The extractive solution was purified by pass-through solid phase extraction column Captiva EMR-Lipid, and the purified liquid was separated on a Agilent Poroshell 120 EC-C18 (2.1 mm×100 mm, 1.9 μm) column. The mobile phase was acetonitrile and 5 mmol/L aqueous ammonium acetate containing 0.05% formic acid. The target compounds were detected by MRM-IDA-EPI mode with external standard method. Results The calibration curves of the 15 kinds of compounds were linear in the concentration range within limits with correlation coefficients between 0.9956 and 0.9996. The limits of detection ranged from 0.62–62.50 μg/kg. The average recoveries of 15 kinds of compounds at 3 different levels ranged from 78.33%–109.51% with accuracy of 0.67%–14.02%. Conclusion The method can be applied to the determination of 15 kinds of chemicals illegally added in prefabricated food with its rapidity, high accuracy and high precision, providing support for quality control and market regulation of prefabricated food.