超高效液相色谱-串联质谱法检测动物源性食品中五氯酚残留

Determination of pentachlorophenol residues in animal derived food by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  五氯酚  混合型强阴离子交换固相萃取柱  超高效液相色谱法-串联质谱法  动物源性食品

英文关键词:pentachlorophenol  mixed anion exchange solid phase extraction column  ultra performance liquid chromatography-tandem mass spectrometry  animal derived food

中文摘要:

      目的 建立超高效液相色谱-串联质谱法检测各类动物源性食品中五氯酚残留的方法。方法 采用三乙胺-乙腈水提取、混合阴离子交换柱净化, 经超高效液相色谱-串联质谱仪检测。研究提取、净化、氮吹、过滤、色谱-质谱分离分析及定性定量等关键控制点, 通过优化提取溶剂的比例、去除氮吹浓缩过程, 最终建立适用于肌肉(猪肉、牛肉、羊肉、鸡肉)、肝脏(猪肝、牛肝、羊肝、鸡肝)、肾脏(猪肾、牛肾、羊肾、鸡肾)、鱼、虾、蟹、贝类、禽蛋(鸡蛋、鸭蛋、鹅蛋、鹌鹑蛋)、牛奶及奶粉中五氯酚残留量的测定方法。结果 五氯酚在0.2~8.0 ng/mL质量浓度范围内线性关系良好(r2>0.99), 检出限(S/N≥3)为0.3 μg/kg, 定量限(limits of quantification, LOQ) (S/N≥10)为1.0 μg/kg。不同基质在LOQ、2LOQ和10LOQ加标水平的回收率均在64.5%~119.0%, 批内、批间相对标准偏差(relative standard deviation, RSD)均小于15%。结论 方法操作简单、准确度高、适用性好, 可满足不同动物性食品中五氯酚残留量的检测。

英文摘要:

      Objective To establish a method for the determination of pentachlorophenol residues in various animal derived foods by ultra performance liquid chromatography-tandem mass spectrometry. Methods Triethylamine acetonitrile water extraction and mixed anion exchange column purification were used, and detected by ultra performance liquid chromatography-tandem mass spectrometer. This article had discussed in detail the key control points such as extraction, purification, nitrogen blowing, filtration, chromatographic-mass spectrometric separation, analysis, and qualitative and quantitative determination. The improved method optimized the proportion of extraction solvents and removed the nitrogen blowing and concentration process. Eventually, a determination method applicable to the residual amounts of pentachlorophenolic acid in muscles (pork, beef, mutton, chicken), livers (pig liver, beef liver, sheep liver, chicken liver), kidneys (pig kidney, beef kidney, sheep kidney, chicken kidney), fish, shrimp, crabs, shellfish, poultry eggs (chicken eggs, duck eggs, goose eggs, quail eggs), milk and milk powder was established. Results The pentachlorophenol were linear in the range of 0.2–8.0 ng/mL with correlation coefficients (r2) higher than 0.99. The limits of detection (S/N≥3) were 0.3 μg/kg, and the limits of quantitation (S/N≥10) were 1.0 μg/kg. The recovery rates of different matrices at LOQ, 2LOQ and 10LOQ spiked levels were all between 64.5% and 119.0%, with intra and inter assay relative standard deviation (RSD) less than 15%. Conclusion The method is simple to operate, highly accurate, and has good applicability, which can meet the detection of pentachlorophenol residues in different animal derived foods.