增强型除脂固相萃取技术结合超高效液相色谱- 串联质谱法测定动物源性食品中五氯酚残留量
目的 建立增强型除脂固相萃取技术结合超高效液相色谱-串联质谱法测定动物源性食品中五氯酚残留量的分析方法。方法 样品经8%三乙胺乙腈:水(80:20, V:V)提取, 经EMR-Lipid固相萃取柱净化, 以 5 mmol/L乙酸铵溶液(含0.1%甲酸)-甲醇作为流动相, Waters ACQUITY BEH C18(50 mm×2.1 mm, 1.7 μm) 进行色谱分离, 在电喷雾负离子模式下, 多反应监测(multiple reaction monitoring, MRM)方式进行测定, 基质匹配外标法定量。结果 猪肉、猪肝、鱼、河虾、蟹、牛奶等6种基质中五氯酚在0.5~10 ng/mL范围内线性良好, 相关系数r>0.997, 方法检出限范围为0.1~0.3 μg/kg, 定量限范围为0.3~0.5 μg/kg, 在1.0、5.0、10.0 μg/kg 3个浓度水平下6种基质中回收率范围为81%~98%, 相对标准偏差范围为1.74%~4.78%之间(n=6)。结论 该方法简单快速、准确可靠, 经济环保, 重复性好, 适用于动物源性食品中五氯酚残留量的测定。
Objective To establish a method for the determination of the pentachlorophenol residue in animal-derived foods by EMR-Lipid-solid-phase extraction ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples was extracted in 8% triethylamine:acetonitrile (80:20, V:V), and purified on the EMR-Lipid-SPE column. The mobile phase was 5 mmol/L ammonium acetate (0.1% formic acid)-methanol. Waters ACQUITY BEH C18 (50 mm×2.1 mm, 1.7 μm) was used for chromatography separation. The pentachlorophenol was analyzed by negative electrospray ionization under the multiple reaction monitoring mode, and matrix matching external standard method was used for quantitative measurement. Results The pentachlorophenol in 6 matrices such as the pork, pork liver, fish, shrimp, crab and milk had good linear relationships in the range of 0.5?10 ng/mL, with correlation coefficient (r) was larger than 0.997. The limites of detection were ranged from 0.1?0.3 μg/kg, the limites of quantification were ranged from 0.3?0.5 μg/kg, and the recoveries at 3 spiked levels (1.0, 5.0, 10.0 μg/kg) were 81%?98%, with the relative standard deviations of 1.74%?4.78% (n=6). Conclusion This method is simple, sensitive, accurate, economical, environmentally safe and reproducible, which is suitable for the determination of the pentachlorophenol residue in animal-derived foods.
标题：增强型除脂固相萃取技术结合超高效液相色谱- 串联质谱法测定动物源性食品中五氯酚残留量
英文标题：Determination of pentachlorophenol residue in animal-origin foods by EMR-Lipid-ultra performance liquid chromatography-tandem mass spectrometry
作者：
夏宝林 江阴市食品安全检测中心
严秋钫 江阴市食品安全检测中心
杨娜 江阴市食品安全检测中心
胡贤伟 江阴市食品安全检测中心
杨佳 无锡微色谱生物科技有限公司
中文关键词:五氯酚残留量,增强型除脂固相萃取,超高效液相色谱-串联质谱法,动物源性食品,
英文关键词:pentachlorophenol residue,EMR-lipid solid-phase extraction,ultra performance liquid chromatography- tandem mass spectrometry,animal-derived foods,
发表日期：2019-05-29
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