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预防医学  2017, Vol. 29 Issue (9): 878-882    DOI: 10.19485/j.cnki.issn1007-0931.2017.09.004
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油炸食品中氯丙醇酯固相萃取GC-MS测定研究
王立媛, 吴平谷, 应英, 王天娇, 胡争艳, 沈向红, 俞莎
浙江省疾病预防控制中心,浙江 杭州 310051
A study on the determination of chloropropanols esters in fried foods by solid-phase extracting method and GC-MS
WANG Li-yuan, WU Ping-gu, YING Ying, WANG Tian-jiao, HU Zheng-yan, SHEN Xiang-hong, YU Sha
Zhengjiang Provincial Center for Disease Control and Prevention,Hangzhou,Zhejiang,310051,China
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摘要 目的 建立油炸食品中氯丙醇酯(包括3-MCPD酯和2-MCPD酯)固相萃取同位素稀释气相色谱-质谱(GC-MS)检测方法,并分析油炸食品中氯丙醇酯水平。方法 在超市、早餐店和街头早餐点采集油炸食品88份,以未检出氯丙醇酯的油炸食品作为空白样品。样品采用溶剂浸提法提取出脂肪,脂肪以甲醇钠-甲醇溶液进行酯键断裂反应,以硅藻土小柱进行固相支持液液萃取净化,净化液经七氟丁酰基咪唑衍生后进行GC-MS检测,以氘代同位素标准品为内标进行内标法定量。采用空白样品的加标回收率评价方法的准确度,以回收率的相对标准偏差(RSD)评价方法的精密度。结果 3-MCPD酯和2-MCPD酯在25~1 000 μg/L浓度范围线性关系良好,相关系数(r)均>0.999 5。3-MCPD酯、2-MCPD酯的检出限均为20 μg/kg。空白样品的脂肪提取物在25、50、100、200 μg/kg水平的加标回收率在89.7%~110.0%之间,RSD均<8.4%。 88份样品中3-MCPD酯和2-MCPD酯检出率分别为81.82%和70.45%,含量范围分别为未检出(ND)~1.65 mg/kg和ND~0.93 mg/kg。结论 该方法适用于油炸食品中氯丙醇酯含量的测定;油炸食品氯丙醇酯污染较为普遍。
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王立媛
吴平谷
应英
王天娇
胡争艳
沈向红
俞莎
关键词 气相色谱-质谱法氯丙醇酯油炸食品    
AbstractObjective To establish an isotope dilution gas chromatography-mass spectrometry(GC-MS) for the determination of chloropropanol esters in fried foods. Methods A total of 88 fried food samples were collected from supermarket,breakfast shop and street breakfast,stalls,the fried food sample with no chloropropanols esters detected was used as the blank sample. Samples were extracted using a solvent extraction method,followed by ester-bond cleavage reaction with sodium methylate-methanol and purification by diatomite solid-supported liquid-liquid extraction column. The derivatives in purified solution was detected by GC-MS after being derivatived with heptafluoro butyrylimidazole. The concentration of chloropropanols esters was quantified by using deuterium isotopes as internal standards. The accuracy of the method for evaluating recovery rate of blank samples was adopted,and the relative standard deviation (RSD) of the recovery rate represents the precision of the method. Results The 3-MCPD ester and 2-MCPD ester had good linear relationship in the concentration range of 25-1 000 g/L(r>0.9995). The detection limits of 3-MCPD ester and 2-MCPD ester were 20 μg/kg. The recovery rate of fat extracts from blank samples at 25,50,100,and 200 μg/kg levels ranged from 89.7% to 103.7%,and RSD<8.4%. The detection rates of 3-MCPD ester and 2-MCPD ester in 88 samples were 81.82% and 70.45% respectively,and the content ranges from not-detected (ND) to 1.65 mg/kg and to 0.93 mg/kg respectively. Conclusion The method is simple,accurate and reliable. It is suitable for the determination of chloropropanol esters in fried foods. There is a certain degree of contamination of chloropropanol esters in fried foods,and this comtamination is quite common.
Key wordsGas chromatography-mass spectrometry    Chloropropanols ester    Fried food
收稿日期: 2016-12-22      修回日期: 2017-02-28      出版日期: 2017-09-30
中图分类号:  R155.58  
基金资助:浙江省科技厅分析测试科技计划项目(2016C37013)
通信作者: 俞莎,E-mail:shyu@zj.cdc.cn   
作者简介: 王立媛,硕士,副主任技师,主要从事理化检验工作
引用本文:   
王立媛, 吴平谷, 应英, 王天娇, 胡争艳, 沈向红, 俞莎. 油炸食品中氯丙醇酯固相萃取GC-MS测定研究[J]. 预防医学, 2017, 29(9): 878-882.
WANG Li-yuan, WU Ping-gu, YING Ying, WANG Tian-jiao, HU Zheng-yan, SHEN Xiang-hong, YU Sha. A study on the determination of chloropropanols esters in fried foods by solid-phase extracting method and GC-MS. Preventive Medicine, 2017, 29(9): 878-882.
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http://www.zjyfyxzz.com/CN/10.19485/j.cnki.issn1007-0931.2017.09.004      或      http://www.zjyfyxzz.com/CN/Y2017/V29/I9/878
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