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当前位置: 首页 > 文章 > 多同位素内标气相色谱-质谱法测定食品中4种氯丙醇含量 食品科学 2013,34 (18) 131-136
Position: Home > Articles > Determination of 4 Kinds of Chloropropanols in Foods by Gas Chromatography-Mass Spectroscopy Coupled with Multi-Isotopic Internal Standard Technique FOOD SCIENCE 2013,34 (18) 131-136

多同位素内标气相色谱-质谱法测定食品中4种氯丙醇含量

作  者：
吴少明;傅武胜;傅海庆;方勤美;华娟
单  位：
福建省人兽共患病研究重点实验室;福建省农业科学院生物技术研究所;福建农林大学金山学院;福建农林大学食品科学学院
关键词：
食品;氯丙醇;基质分散固相萃取法;同位素稀释技术;气相色谱-质谱法
摘  要：
采用多同位素内标法,结合七氟丁酰基咪唑(HFBI)衍生化的气相色谱-质谱(GC-MS)联用技术,建立了食品中4种氯丙醇含量的检测方法。对比了不同来源HFBI衍生试剂的作用性能,对定量内标物和校正标准的选择进行了比较。结果表明:仅用2种同位素内标(3-氯-1,2-丙二醇-d5(或2-氯-1,3-丙二醇-d5)和1,3-二氯-2-丙醇-d5)校正,同样可达到准确测定食品中4种氯丙醇含量的要求;若采用3-氯-1,2-丙二醇(3-MCPD)为标准物定量测定2-氯-1,3-丙二醇(2-MCPD)时,所得2-MCPD结果偏低,仅为以2-MCPD为标准物定量结果(真实值)的52.1%~77.8%。在最佳条件下进行了方法学指标的系统验证。4种氯丙醇的最低检出限为2.5~10μg/kg;在100~2000ng范围内,氯丙醇与内标物峰面积的比值和质量呈线性关系(R2>0.9990)。以酱油和方便面调料粉为基质,进行100、200、400μg/kg三个水平的加标回收实验,4种氯丙醇的回收率均值为90.1%~107%,相对标准偏差(RSD)为3.37%~10.4%(n=6),均满足痕量分析的要求。
译  名：
Determination of 4 Kinds of Chloropropanols in Foods by Gas Chromatography-Mass Spectroscopy Coupled with Multi-Isotopic Internal Standard Technique
作  者：
WU Shao-ming;FU Wu-sheng;FU Hai-qing;FANG Qin-mei;HUA Juan;Fujian Provincial Key Laboratory of Zoonosis Research,Center for Disease Control and Prevention;Fujian Inspection and Research Institute for Product Quality;College of Jinshan,Fujian Agriculture and Forestry University;Biotechnology Research Institute,Fujian Academy of Agricultural Sciences;College of Food Science,Fujian Agriculture and Forestry University;
关键词：
food;;chloropropanol;;dispersion matrix solid-phase extraction;;isotopic internal standard technique;;gas chromatography-mass spectrometer(GC-MS)
摘  要：
An analytical method was developed to determine 4 kinds of chloropropanols in foods using gas chromatography mass spectrometer coupled with the multi-isotopic internal standard technique.The performance difference between different brands of HFBI as a derivativization reagent and internal standard selection for quantification were discussed.Under the optimal conditions,the limits of detection(LOD) were 2.5–10 μg/kg for 4 kinds of chloropropanols.According to the internal standard calibration,an excellent linearity between 100 ng and 2000 ng of chloropropanols(R2 > 0.9990) was obtained.When chloropropanols were spiked at levels of 100,200,400 mg/kg in soy sauce and seasoning powder of instant noodles,the average recovery rates were 90.1%–107%,with relative standard deviation(RSD) of 3.37%–10.4%(n = 6).The application of only 2 kinds of internal standards(chloropropane-1,2-diol-d5 or 2-chloropropane-1,3-diol-d5 and 1,3-dichloro-2-propanol-d5) can reveal accurate and precise determination for 4 kinds of chloropropanols.When 3-chloropropane-1,2-diol(3-MCPD) was used to calibrate 2-MCPD in foods,the level of 2-chloropropane-1,3-diol(2-MCPD) was only 52.1%–77.8% of the real content.

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