固相萃取-气相色谱-质谱法测定酸奶中氨基甲酸乙酯  

Determination of ethyl carbamate in yogurt by solid phase extraction-gas chromatography-mass spectrometry

作　　者：雒丽娜[1] 王颖[1] 张妮娜[1] 马腾蛟[1] 李疆[1] 段鹤君[1] 

机构地区：[1]北京市疾病预防控制中心,北京100013

出　　处：《中国卫生检验杂志》2015年第18期3070-3071,共2页Chinese Journal of Health Laboratory Technology

摘　　要：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 ethyl carbamate content in yogurt by gas solid - phase ex- traction combined with chromatography- mass spectrometry（ GC - MS）. Methods 0.1 g yogurt sample was weighed and the ethyl earbmnate - d5 was added into the sample as the internal standard. Then the sample was extracted with acetonitrile and pu- rified with florisil solid phase extraction column. After concentrated the eluate was determined by GC - MS. Results The ethyl carbamate showed good linear relation in the range of 20 ng/ml -800 ng./ml, the average recovery rate at three additive level 200.0 ng/g, 100.0 ng,/g and 40.0 ng/g was 104.0% , 106.4% and 91.2%, respectively, and RSD was 2.28%, 2.55% and 4.77%, respectively. The limit of quantitation was 10.0 μg/kg. Conclusion The method has good purification effect, and the sensitivity and accuracy of the method are all satisfied the detection requirements. The method has the advantages of ease op- eration, less interference, rapidity, accuracy and other characteristics, and it is suitable for determination of ethyl carbamate in yogurt products.

关 键 词：酸奶 氨基甲酸乙酯 内标法 固相萃取 气相色谱-质谱法 

分 类 号：O657.63[理学—分析化学]