气相色谱法检测汤料中氯丙醇类化合物
Gas Chromatographic Determination of Chloropropanols in Stocks
摘 要
应用毛细管柱-气相色谱法测定汤料中氯丙醇类化合物.汤料试样中氯丙醇类化合物在索氏抽取器中用乙醚萃取,于萃取液中通入氮气吹干乙醚,残留物用每次1 mL甲醇萃取两次以净化氯丙醇类化合物.收集并合并甲醇萃取液,蒸发除去甲醇后用N,O-双(三甲基硅烷)-三氟乙酰胺进行衍生化,所得衍生物经毛细管色谱柱分离,用氢火焰离子化检测器(FID)检测,方法的检出限为0.01 mg·kg-1.对精密度及回收率作了试验,得到的回收率在95%~102%之间,RSD(n=5)值小于4.5%.
毛细管色谱柱
氯丙醇类化合物
汤料
Gas chromatography
Chloropropanols
Capillary column
Stocks
Abstract
Gas chromatography with capillary column was applied to the determination of chloropropanols in stocks.Chloropropanols in the stock sample was extracted with ethyl ether using Soxhlet apparatus,and the ethyl ether was evaporated by nitrogen stream.The chloropropanols were then purified by extraction with methanol twice in 1 mL portions.The extracts were collected and methanol was evaporated,and derivatized with N,O-bis(trimethylsilyl)-trifluoroacetamide (BSTFA).The derivatives was separated on the capillary chromatographic column and determined by flame ionization detection.Detection limit of the method was 0.01 mg·kg-1.Tests for recovery and precision were done giving values of recovery in the range from 95% to 102%,and RSD′s (n=5) less than 4.5%.
中图分类号 O657.7
所属栏目 工作简报
基金项目
收稿日期 2006/9/2
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备注张明霞(1971-),女,河北省泊头市人,副教授,硕士,主要从事化学教学和食品检测研究工作.
引用该论文: ZHANG Ming-xia,CHEN Xue-qiao,ZHOU Jian-ke. Gas Chromatographic Determination of Chloropropanols in Stocks[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2007, 43(11): 953～955
张明霞,陈雪桥,周建科. 气相色谱法检测汤料中氯丙醇类化合物[J]. 理化检验－化学分册, 2007, 43(11): 953～955
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参考文献
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【7】Plantinga W J,Van Toon W G,Van Der Stegen G H D.Determination of 3-chloropropane-1,2-diol in liquid hydrolysed vegetable protein by capillary gas chromatography with flame ionization detection[J].J Chromatogr,1991,555:311．(上接第952页)
【8】Garcya-Marino M,Rivas-Gonzalo J,Garcya-Marino C.Recovery of catechins and proanthocyanidins from winery by-products using subcritical water extraction[J].Analytica Chimica Acta,2006,563:44-50．
【9】Hashimoto S,Watanabe K,Nose K,et al.Remediation of soil contaminated with dioxins by subcritical water extraction[J].Chemosphere,2004,54:89-96．
【10】McGowin A E,Adom K K,Obubuafo A K.Screening of compost for PAHs and pesticides using static subcritical water extraction[J].Chemosphere,2001,45:857-864．
【11】Hawthorne S B,Trembley S,Moniot C L,et al.Static subcritical water extraction with simultaneous solid-phase extraction for determining polycyclic aromatic hydrocarbons on environmental solids[J].Journal Chromatogr A,2000,886:237-240．
【12】王琳玲,杨海,陆晓华.活性碳纤维对硝基酚的吸附行为和应用研究[J].工业水处理,2003,23(2):23-25．
【13】Crespin M A,Gallego M,Valcarcel M.A semiautomatic module for the direct leaching and determination of sixteen phenols in soils[J].Anal Chem,1999,71:2687-2690．
【14】US EPA Method 8041-1996,phenols by gas chroma tography[S].
【15】US EPA Method 8081A 1996,organochlorine pesticides by gas chromatography[S].
【2】Barrry S Lynch,Douglals W Bryant,Graham J Hook,et al.Carcinogenicity of monochloro-1,2-propanediols (a-chlorohydrin,3-MCPD)[J].International Journal of Toxicology,1998,17:47．
【3】高文宏,李国基,于淑娟,等.水解植物蛋白[J].食品科学,2000,21(2):167．
【4】Ver Bergen C A,Collier P D,Cromie D D O,et al.Determination of chloropropanols in protein hydrolysates[J].J Chromatogr,1992,589:109．
【5】Kissa E.Determination of 3-chloropro -panediol and related dioxolanes by gas chromatography[J].J Chromatogr,1992,605:134．
【6】张思群,王志远,许 毅.调味品中氯丙醇的GC/ECD和GC/MS/MS衍生化检测方法研究及应用[J].分析科学学报,2003,19(6):543．
【7】Plantinga W J,Van Toon W G,Van Der Stegen G H D.Determination of 3-chloropropane-1,2-diol in liquid hydrolysed vegetable protein by capillary gas chromatography with flame ionization detection[J].J Chromatogr,1991,555:311．(上接第952页)
【8】Garcya-Marino M,Rivas-Gonzalo J,Garcya-Marino C.Recovery of catechins and proanthocyanidins from winery by-products using subcritical water extraction[J].Analytica Chimica Acta,2006,563:44-50．
【9】Hashimoto S,Watanabe K,Nose K,et al.Remediation of soil contaminated with dioxins by subcritical water extraction[J].Chemosphere,2004,54:89-96．
【10】McGowin A E,Adom K K,Obubuafo A K.Screening of compost for PAHs and pesticides using static subcritical water extraction[J].Chemosphere,2001,45:857-864．
【11】Hawthorne S B,Trembley S,Moniot C L,et al.Static subcritical water extraction with simultaneous solid-phase extraction for determining polycyclic aromatic hydrocarbons on environmental solids[J].Journal Chromatogr A,2000,886:237-240．
【12】王琳玲,杨海,陆晓华.活性碳纤维对硝基酚的吸附行为和应用研究[J].工业水处理,2003,23(2):23-25．
【13】Crespin M A,Gallego M,Valcarcel M.A semiautomatic module for the direct leaching and determination of sixteen phenols in soils[J].Anal Chem,1999,71:2687-2690．
【14】US EPA Method 8041-1996,phenols by gas chroma tography[S].
【15】US EPA Method 8081A 1996,organochlorine pesticides by gas chromatography[S].
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