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目的建立酸奶中氨基甲酸乙酯的固相萃取-气相色谱-质谱检测方法。方法称取1.0 g的酸奶样品,加入氨基甲酸乙酯-d5内标溶液后,采用乙腈提取样品,提取液经佛罗里硅土固相萃取柱净化,净化液浓缩定容后用气相色谱-质谱法测定。结果氨基甲酸乙酯在20 ng/ml~800 ng/ml时呈良好的线性关系,3个加标水平200.0 ng/g、100.0 ng/g和40.0 ng/g的平均回收率分别为104.0%、106.4%和91.2%,相对标准偏差(RSD)分别为2.28%、2.55%和4.77%,定量限为10.0μg/kg。结论方法净化效果好,检测灵敏度、准确度均满足检测要求,具有操作简单、干扰少、快速、准确可靠等特点,适用于酸奶中氨基甲酸乙酯的检测。
Objective To establish a method for the determination of urethane in yoghurt by gas chromatography-mass spectrometry. Method Weigh 1.0 g of yogurt samples, add ethyl carbamate-d5 internal standard solution, the sample was extracted with acetonitrile, the extract was purified by Florisil solid-phase extraction column, the purification solution was concentrated and determined by gas chromatography - Mass spectrometry. The results showed that urethane showed a good linearity at 20 ng / ml ~ 800 ng / ml. The average recoveries of three spiked levels of 200.0 ng / g, 100.0 ng / g and 40.0 ng / g were 104.0% The relative standard deviations (RSDs) were 2.28%, 2.55% and 4.77%, respectively. The limit of quantification was 10.0μg / kg. Conclusion The method has good purification effect, detection sensitivity and accuracy meet the test requirements. It has the characteristics of simple operation, less interference, fast, accurate and reliable. It is suitable for the detection of urethane in yogurt.