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首页> 外文会议>American Society for Mass Spectrometry Conference on Mass Spectrometry and Allied Topics >Determination of 3-chloro-1,2-propanediol in soy sauce samples with supported liquid extraction and GC-MS
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Determination of 3-chloro-1,2-propanediol in soy sauce samples with supported liquid extraction and GC-MS

机译：用负载液提取和GC-MS测定酱油样品中3-氯-1,2-丙二醇

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This paper presents a method for the determination of 3-chloro-1, 2-propanediol (3-MCPD) in soy sauce samples, which prepared by a new method of supported liquid extraction (SLE) followed by analysis with gas chromatography-mass spectrometry (GC/MS). Soy sauce samples were extracted and prepared by supported liquid extraction (SLE) cartridges, then the analyte was eluted by ethyl acetate and derivatized with N-(heptafluoro-n-butyryl)-imidazole (HFBI). The derivatized samples were washed by saturated solution of sodium chloride, and determined by GC/MS with a capillary column (DA-5MS, 30 m × 0.25 mm × 0,25μm). In this paper, the detection limit of 3-MCPD was found to be　　 0.3 μg/kg. Calibration curve for 3-MCPD from 1 to 1000 ng/mL was highly linear with a correlation coefficient 0.9993. The mean recoveries of spilked samples at the level of 5 μg/kg and 200 μg/kg were found in a range from 83.6% to 98.9%. The relative standard deviations (n = 5) were from 3.18% to 4.36%. This method was validated to be safe, ffective and sensitive for the determination of 3-MCPD in a large number of soy sauce samples.
机译：本文介绍了在酱油样品中测定3-氯-1,2-丙二醇（3-MCPD）的方法，该样品通过支持液体萃取（SLE）的新方法，然后用气相色谱 - 质谱分析（GC / MS）。通过负载液萃取（SLE）盒来提取和制备酱油样品，然后通过乙酸乙酯洗脱分析物并用N-（庚二氟-N-丁酰基） - 咪唑（HFBI）衍生化。通过饱和氯化钠溶液洗涤衍生化样品，并通过GC / MS与毛细管柱（DA-5ms，30m×0.25mm×0,25μm）测定。在本文中，发现3-MCPD的检出限为0.3μg/ kg。 3-MCPD的校准曲线从1至1000ng / ml具有高度线性，具有相关系数0.9993。在5μg/ kg和200μg/ kg的水平下的平均刺激样品的回收率在83.6％至98.9％的范围内。相对标准偏差（n = 5）为3.18％至4.36％。验证该方法是安全，效果和敏感的，用于在大量酱油样品中测定3-MCPD。

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