刘宇航,于寒冰,杨红菊,马啸,温雅君,孙志伟,习佳林,熊慧勤,肖志勇.高效液相色谱-四极杆-飞行时间质谱法快速筛查蔬菜中124种药物残留[J].食品安全质量检测学报,2024,15(16):175-184 |
高效液相色谱-四极杆-飞行时间质谱法快速筛查蔬菜中124种药物残留 |
Rapid screening of 124 Pharmaceuticals and Personal Care Products (PPCPs) in vegetables by LC-QTOF/MS |
投稿时间:2024-03-22 修订日期:2024-08-29 |
DOI: |
中文关键词: 药品残留(PPCPs) 蔬菜 高效液相色谱-四极杆-飞行时间质谱(LC-QTOF/MS) 快速筛查 |
英文关键词:Pharmaceuticals and Personal Care Products (PPCPs) Vegetables High performance liquid chromatography-Quadrupole-time-of-flight mass spectrometry (LC-QTOF/MS) Rapid screening |
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中文摘要: |
目的 本文基于高效液相色谱-四极杆-飞行时间质谱(High performance liquid chromatography quadrupole time-of-flight mass spectrometry,LC-QTOF/MS)建立蔬菜中124种药物和个人护理品(Pharmaceuticals and personal care products,PPCPs)的同时快速筛查、确证和定量分析方法。方法 样品经过10 mL乙腈提取,改进QuEChERS方法净化,电喷雾电离,正离子(Product-Ion扫描模式检测)扫描,基质匹配外标法定量;建立一级精确质量数据库、色谱保留时间和二级质谱库,实现蔬菜中124种目标污染物的快速筛查和确证。结果 在0.005~0.2 mg/kg质量浓度范围内,124种目标化合物的线性关系良好(r > 0.99)。多种蔬菜基质中0.01、0.05、0.2 mg/kg的3个加标水平下平均回收率分别为63.2%~108.5%,65.6%~117.2%,62.7%~105.6%,相对标准偏差(RSD)分别为1.6%~8.1%,1.7%~9.5%,1.9%~8.9%。满足痕量分析要求,基质干扰效应消除效果较好,该方法具有良好的净化效果。结论 该方法具有操作简便、耗时短、灵敏度高、稳定性好的优点,适用于蔬菜基质中PPCPs的筛查检测及定量分析,对蔬菜质量安全的快速筛查具有技术支撑意义。 |
英文摘要: |
Objective To establish a method for simultaneous screening, confirmation and quantitative analysis of 124 pharmaceuticals and personal care products (PPCPs) in vegetables based on high performance liquid chromatogre-quadrupole time-of-flight mass spectrometry (LC-QTOF/MS). Methods The samples were extracted by 10 mL acetonitrile, purified by QuEChERS, electrospray ionization, positive Ion (product-ion scan pattern detection) scanning, and quantified by matrix matching external standard method. The primary accurate mass database, chromatographic retention time and secondary mass spectrometry database were established to rapidly screen and confirm the existence of 124 targeted pollutants in vegetables. Results In the mass concentration range of 0.005~0.2 mg/kg, the linear relationship of 124 compounds was good (r > 0.99). The average recoveries at 0.01, 0.05 and 0.2 mg/kg were 63.2%~108.5%,65.6%~117.2%,62.7%~118.6%,and the relative standard deviations (RSD) were 1.6%~8.1%,1.7%~9.5%,1.9%~8.9%. The method meets the requirements of trace analysis and eliminates the interference of vegetable matrix. Conclusion The method is simple, time-saving, sensitive and stable, which is suitable for the screening and quantitative analysis of PPCPs in vegetables. |
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