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建立了气相色谱-质谱法检测动物源性食品中葚孢菌素残留量的方法。采用环己烷-二氯甲烷(体积比为9:1)振荡提取,中性氧化铝固相萃取柱净化,气相色谱-质谱法进行测定,选择离子监测模式检测。通过方法优化,确定方法检出限为0.01mg/kg(S/N=10),在0.005~1mg/kg范围内线性关系良好(R2=0.9999)。在0.01、0.05、0.10mg/kg 3个添加水平下,葚孢菌素的添加回收率在70.5%~102.1%,相对标准偏差(RSD)为3.4%~5.7%。
A gas chromatography-mass spectrometry method was developed for the determination of carbamazepine residues in animal-derived foods. The sample was extracted with cyclohexane-dichloromethane (9: 1 by volume), cleaned up by neutral alumina solid-phase extraction (SPE) cartridge and analyzed by gas chromatography-mass spectrometry. Through the method optimization, the detection limit was 0.01mg / kg (S / N = 10). The linearity was good in the range of 0.005 ~ 1mg / kg (R2 = 0.9999). At 3 levels of 0.01, 0.05 and 0.10 mg / kg, the recoveries of carbamazepine were between 70.5% and 102.1% with relative standard deviations (RSDs) of 3.4% -5.7%.