摘要
建立一种快速测定鸡精中3-氯-1,2-丙二醇(3-MCPD)和1,3-二氯-2-丙醇(1,3-DCP)质量浓度的衍生化毛细管柱气相色谱法。采用基质固相分散萃取法(MSPD),以硅藻土(Extrelut TM20)为吸附剂,鸡精样品用正己烷淋洗净化后用乙醚提取,用七氟丁酰咪唑(HFBI)衍生,经毛细管气相色谱柱DB-5(30m×0.32mm×0.25μm)分离,电子捕获检测器测定,外标法定量。3-MCPD和1,3-DCP均在0.010～0.250mg/L质量浓度范围内线性关系良好,线性相关系数分别为0.999 1和0.999 3;加标水平为0.05,0.10和0.20mg/kg时,3-MCPD的回收率在95.7%～102.2%之间,1,3-DCP的回收率在94.5%～99.3%之间,相对标准偏差均小于5.0%。3-MCPD和1,3-DCP的定量限均为0.01mg/kg。该法操作简单、快捷,灵敏度高,试验结果准确可靠,适用于鸡精样品中2种氯丙醇的同时测定。
A gas chromatographic method was developed for the determination of 3-chloropropane-1,2- diol （3-MCPD） and 1, 3-dichloropropan-2-ol （ 1, 3-DCP） in chicken essence. Matrix solid-phase dispersion extraction（MSPD） was used to the extraction and clean-up of chloropropanols in chicken essence. Samples were eluted from extrelut chromatography column with n-hexane. Chloropropanols was extracted by diethyl ether, derivatised by heptafluorobutyrylimidazole（HFBI） and analyzed by gas chromatography, using DB-5（30 m× 0.32 mm × 0.25 μm） capillary column for separation and electron capture detector（ECD）for detection. The method of external standards was used in determination. Good linear relationships of the two analytes are obtained over the range of 0. 010-0. 250 mg/L,with correlation coefficients of 0. 999 I and 0. 999 3,respectively. Average recoveries of 3-MCPD and 1,3-DCP from chicken essence spike at three concentration levels of 0.05, 0. 10 and 0. 20 mg/kg ranging from 95. 7% to 102. 2%and 94. 5%to 99. 3%, respectively. Both relative standard deviations are less than 5. 0% and both the limit of quantitation（LOQ） are 0.01 mg/kg. The proposed method is easy to opera, rapid and accurate for precise determination of 3-MCPD and 1,3-DCP in chicken essence with satisfactory results.
出处
《浙江科技学院学报》
CAS
2013年第1期33-37,共5页
Journal of Zhejiang University of Science and Technology
