亲水液相色谱-串联质谱法测定羊肌肉组织中安乃近代谢物的残留量

建立了羊肌肉组织中安乃近4 种主要代谢物--4-甲氨基安替比林、4-氨基安替比林、4-甲酰氨基安替比林和4-乙酰氨基安替比林的亲水液相色谱-串联质谱分析方法。肌肉样品均质后，用体积分数为5%的氨水乙腈提取，提取液用Cleanert PSA初步净化，60 ℃氮气吹干,乙腈复溶后过MAX（SPE）柱净化，采用亲水液相色谱-串联质谱测定，4 种物质均采用外标法定量。结果显示：4-甲氨基安替比林、4-甲酰氨基安替比林和4-乙酰氨基安替比林在添加量为4～200 μg/kg范围内线性良好；4-氨基安替比林在添加量为40～2 000 μg/kg范围内线性良好。在5、50、100、1 000 μg/kg 4 个添加量，回收率在75.02%～116.2%范围内。日内变异系数为1.63%～15.12%（n=5），日间变异系数均小于11%（n=15）。4-甲氨基安替比林、4-甲酰氨基安替比林和4-乙酰氨基安替比林的检测限均为0.5 μg/kg，4-氨基安替比林的检测限为5 μg/kg。该方法灵敏度高、重复性好，适用于羊肌肉组织中安乃近4 种主要代谢物的大批量样品检测。

Simultaneous Determination of Residues of Four Dipyrone Metabolites in Goat Muscle by Hydrophilic Interaction Liquid Chromatography-Mass Spectrometry

A hydrophilic interaction liquid chromatography-mass spectrometry (HILIC-MS) method was developed for
the determination of four dipyrone metabolites, namely 4-methylaminoantipyrine (MAA), 4-aminoantipyrine (AA),
4-formylaminoantipyrine (FAA), and 4-acetylaminoantipyrine (AAA) in goat muscle. These metabolites were extracted with
acetonitrile mixed with 5% ammonia. The extracts were cleaned up with Cleaner PSA, and then blow-dried by nitrogen gas,
re-dissolved in acetonitrile and re-cleaned up using MAX (SPE) cartridge. After chromatographic separation, the analytes were
quantified by the external standard method. The calibration curves were linear between 4 and 200 μg/kg matrix equivalent
concentrations for MAA, FAA, and AAA, and between 40 and 2 000 μg/kg for AA. The mean recoveries in blank samples
at four spike levels (5, 50, 100, and 1 000 μg/kg) ranged between 75.02% and 116.2%. The intra-day coefficient of variation
(CV) was 1.63% to 15.12% (n = 5), and the inter-day CV was less than 11% (n = 15). The detection limits were 0.5 μg/kg
for MAA, FAA and AAA and 5 μg/kg for AA. The proposed method is sensitive and repeatable, allowing analysis of a large
number of samples in a working day.