食品科学

• 分析检测 • 上一篇    下一篇

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

吴少明,傅武胜,傅海庆,方勤美,华 娟   

  1. 1.福建省人兽共患病研究重点实验室,福建省疾病预防控制中心,福建 福州 350001;
    2.福建省产品质量检验研究院,福建 福州 350002;3.福建农林大学金山学院,福建 福州 350002;
    4.福建省农业科学院生物技术研究所,福建 福州 350003;5.福建农林大学食品科学学院,福建 福州 350002
  • 出版日期:2013-09-25 发布日期:2013-09-27

Determination of 4 Kinds of Chloropropanols in Foods by Gas Chromatography-Mass Spectroscopy Coupled with Multi-Isotopic Internal Standard Technique

WU Shao-ming,FU Wu-sheng,FU Hai-qing,FANG Qin-mei,HUA Juan   

  1. 1. Fujian Provincial Key Laboratory of Zoonosis Research, Center for Disease Control and Prevention, Fuzhou 350001, China;
    2. Fujian Inspection and Research Institute for Product Quality, Fuzhou 350002, China;
    3. College of Jinshan, Fujian Agriculture and Forestry University, Fuzhou 350002, China;
    4. Biotechnology Research Institute, Fujian Academy of Agricultural Sciences, Fuzhou 350003, China;
    5. College of Food Science, Fujian Agriculture and Forestry University, Fuzhou 350002, China
  • Online:2013-09-25 Published:2013-09-27

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。

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

Abstract:

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.

Key words: food, chloropropanol, dispersion matrix solid-phase extraction, isotopic internal standard technique, gas chromatography-mass spectrometer (GC-MS)