超高效液相色谱-电喷雾串联质谱测定动物源食品中五氯酚的残留量

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

采用固相萃取净化样品,结合液相色谱-三重四极杆串联质谱技术(LC-MS/MS),在负离子扫描模式下,建立了3种动物源食品(鸡肉、鱼肉、虾肉)中五氯酚残留的检测方法。优化的仪器检测条件为:5 mmol/L乙酸铵溶液和甲醇作为流动相,梯度洗脱。选用0. 02 mol/L盐酸-乙腈溶液作为提取溶剂,经WAX固相萃取小柱净化处理后,在0. 001,0. 004和0. 05 mg/kg3个添加水平下,五氯酚在鸡肉、鱼肉和虾肉中的回收率分别为88. 8%～98. 8%,93. 1%～104. 3%和89. 2%～98. 4%,相对标准偏差(RSD)分别为6. 2%～7. 9%,3. 7%～5. 1%和7. 1%～9. 2%。五氯酚在3种样品中的定量限均为0. 001 mg/kg。本方法可用于动物源食品中五氯酚的残留检测。

A rapid and sensitive method based on solid phase extraction using liquid chromatographytandem mass spectrometry(LC-MS/MS)in negative ion scanning was developed for the residue detection of pentachlorophenol in three animal-origin foods(chicken,fish and prawn).When using methanol-5 mmol/L ammonium acetate as the mobile phase,gradient elution resulted in the best chromatographic resolution and sensitivity.When 0.02 mol/L hydrochloric acid-acetonitrile solution was used as the extraction solvent,the samples were purified by WAX solid phase extraction cartridge,at the spiked levels of 0.001,0.004 and 0.05 mg/kg.The average recoveries of pentachlorophenol were 88.8%-98.8%,93.1%-104.3%and 89.2%-98.4%,with relative standard deviations of6.2%-7.9%,3.7%-5.1%and 7.1%-9.2%in chicken,fish and prawn,respectively.The limit of quantification(LOQ)was 0.001 mg/kg,which was defined as the lowest spiking level with satisfactory recovery results.This established method was suitable for the residual detecting of pentachlorophenol in animal-origin foods.