酱油中双氯丙醇的顶空固相微萃取-气相色谱-质谱法测定
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苗虹女副研究员 研究方向为食品中化学污染物 监测与暴露评估 E-mail:miaohong0827@ 163.Com

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卫生公益性行业科研专项经费(200902009);卫生部法监司食品卫生标准制修订项目(20070162)


Determination of Dichloropropanols by Head-Space Solid Phase Micro-Extraction (HS-SPME) Using Gas Chromatography – Mass Spectrometry (GC-MS) in Soy Sauce
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    摘要:

    目的 建立酱油中双氯丙醇(1,3-dichloro-2-propanol即1,3-DCP和2,3-dichloro-1-propanol即2,3-DCP)的顶空固相微萃取-气相色谱-质谱法的测定方法.方法 采用涂层膜厚为75 μm的CarboxenTM/聚二甲基硅氧烷(CAR/PDMS)的固相微萃取纤维,在50℃水浴中对酱油样品直接进行萃取30 min后移至气相色谱质谱联用仪上,经DB-WAX毛细管柱(30 m×0.25 mm×0.25μm)分离后质谱测定,以d5-1,3-DCP为内标进行内标法定量.结果 酱油样品中1,3-DCP及2,3-DCP的舍量与1,3-DCP及2,3-DCP和d5-1,3-DCP内标的峰面积比呈良好的线性关系,线性范围为5~160μg/kg,相关系数大于0.998.以空白酱油为基质做了3个添加水平(5、20和50μg/kg)的加标回收实验,回收率在82.3%~113.4%之间,相对标准偏差(RSD,n=7)在2.5%~10.6%之间,方法的精密度和准确度良好.酱油中1,3-DCP和2,3-DCP的检测限分别为2和0.5μg/kg.对酱油样品进行了测定,结果满意.结论 该方法简单、快速、准确、灵敏度高、无需使用有机溶剂,适用于酱油样品中双氯丙醇的直接测定.

    Abstract:

    Objective To establish a GC-MS method for the detection of 1,3-dichloro-2-propanol(1, 3-DCP)and 2, 3-dichloro-1-propanol(2, 3-DCP)in soy sauce by using a head-space solid phase micro-extraction device. Method Extracting 1, 3-DCP and 2, 3-DCP from soy sauce in 50 ?C water bath for 30 min with a CarboxenTM/Polydimethylsiloxane(CAR/PDMS,75μm)fiber. The fiber was then transferred to the injection port of GC – MS to allow the analyte absorbed and separated by DB – WAX capillary column (30 m×0.25 mm×0.25 μm) and detected by mass spectrometry. Using d5-1,3-DCP as internal standard for quantification. Results The linear range for 1, 3-DCP and 2, 3-DCP was 5-160 μg/kg, and the detection limits were 2.0 μg/kg and 0.5 μg/kg respectively. The recoveries of standard addition at 5μg/kg, 20μg/kg and 50μg/kg were in the range of 82.9 % - 103.0 %, and the relative standard deviations (RSD, n=7) were in the range of 2.5 % - 10.6 %. Satisfactory results were obtained in the detection of 1, 3-DCP and 2, 3-DCP in soy sauce samples. Conclusion The method is simple, fast, accurate, sensitive, and suitable for the determination of 1, 3-DCP and 2, 3-DCP in soy sauce.

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苗虹,张磊,赵云峰,吴永宁.酱油中双氯丙醇的顶空固相微萃取-气相色谱-质谱法测定[J].中国食品卫生杂志,2010,22(3):199-205.

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  • 收稿日期:2010-03-15
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