高效液相色谱-串联质谱法检测猪肉中3-甲基喹喔啉-2-羧酸残留

建立了高效液相色谱-串联质谱同时定量和确证猪肉中3-甲基喹喔啉-2-羧酸(MQCA)残留量的检测方法。试样用0.3mol/L盐酸溶液水解提取,加入乙腈和乙酸乙酯萃取,再用0.1mol/L氢氧化钠溶液反萃取,阴离子交换固相萃取柱净化,经AgilentEclipsePlusC18柱(50mm×3.0mm,1.8μm)分离,采用液相色谱-串联质谱仪检测,基质匹配添加标准曲线定量。MQCA在1.0~50μg/L范围内线性相关系数大于0.99,在0.5、1.0、5.0μg/kg加标水平下其回收率为90.5%~119.6%,相对标准偏差为3.14%~4.22%。方法可用于猪肉中MQCA残留量的快速定量和确证检测。

Determination of 3-methyl-quinoxaline-2-carboxylic acid residue in pork by high performance liquid chromatography-tandem mass spectrometry

A method was developed for the simultaneous quantitative and confirmatory determination of 3-methylquinoxaline-2-carboxylic acid (MQCA) residues in pork by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was hydrolyzed with 0.3 mol/L hydrochloric acid solution, and MQCA was extracted by water bath oscillation. MQCA was first extracted with acetonitrile and ethyl acetate and then re-extracted from the extraction solution with 0.1 mol/L sodium hydroxide solution. Then MQCA was purified by an anion exchange solid phase extraction column. The chromatographic separation was performed using an Agilent Eclipse Plus C18 column (50 mm×3.0 mm, 1.8 μm). The quantitative analysis was performed by the matrix matching addition method. The correlation coefficient of MQCA in the range of 1.0-50 μg/L was greater than 0.99. The recovery was 90.5%-119.6% at the spiked levels of 0.5, 1.0 and 5.0 μg/kg, and the relative standard deviation was 3.14%-4.22%. The method can be used for the rapid quantitative determination of 3-methylquinoxaline-2-carboxylic acid residues in pork.