双[2,4,6-三氯苯基]草酸酯-过氧化氢体系流动注射化学发光法检测地沟油中的胆固醇  

Determination of Cholesterol in Hogwash Oil by Flow Injection Chemiluminescence with Bis(2,4,6-trichlorophenyl) oxalate-Hydrogen Peroxide System

作　　者：肖虎勇[1] 陈佳[1] 魏国芬[1] 胡芹芹[1] 艾永青[1] 韩韵[1] 周兴旺[1] 吕鉴泉[1] 

机构地区：[1]湖北师范学院污染物分析与资源化技术湖北省重点实验室,黄石435002

出　　处：《分析化学》2013年第3期432-435,共4页Chinese Journal of Analytical Chemistry

基　　金：湖北省自然科学基金重大项目(No.2010CDA061);湖北省教育厅创新团队项目和重点项目(No.D200922005);污染物分析与资源化技术湖北省重点实验室开放基金(No.KY2010M03)资助

摘　　要：基于胆固醇和冰乙酸的反应物与硫酸铁铵生成的紫色化合物能有效抑制双[2,4,6-三氯苯基]草酸酯(Bis(2,4,6-trichlorophenyl)oxalate,TCPO)-H2O2-咪唑化学发光反应,建立了流动注射-化学发光联用检测胆固醇的方法。对流动注射、化学发光等实验参数进行了优化。当咪唑浓度为0.001 mol/L,H2O2浓度为0.3 mol/L,TCPO浓度为1.0×10"3mol/L,主副蠕动泵转数分别为20和15 r/min时,体系具有最强的化学发光。在优化的实验条件下,测定胆固醇的线性范围为8.6×10"6～2.2×10"4mol/L;检出限(S/N=3)为2.5×10"6mol/L;相对标准偏差(RSD,n=11,c=6.5×10"5mol/L)为1.5%。不同加标水平下的加标回收率为95.0%～105.0%;相对标准偏差(n=6)小于3.6%。本方法已应用于地沟油中胆固醇的测定,结果令人满意。Based on the inhibiting effect of product of cholesterol-glacial acetic acid-ammonium ferric sulfate on the bis （2,4,6-trichlorophenyl） oxalate （ TCPO）-H2O2-imidazole chemiluminescence （CL） reaction, a flow-injection coupling with indirect CL detection method for the determination of cholesterol was developed. The key experimental parameters for flow injection and CL were respectively optimized. The optimal conditions of CL system were 0. 001 mol/L imidazole, 0.3 mol/L H202 and 1.0xl0-3 mol/L TCPO, and peristaltic pump was 20 r/min and that of sub-peristaltic pump was 15 r/min. Under the optimum conditions, the rela- tive CL intensity is linearly proportional to the concentration of cholesterol from 8.6x 10-6-2. 2x 104 mol/L （R=O. 9988）, the detection limit （S/N=3） turned out to be 2.5x10~ mol/L. For the analysis （n= 11 ） of 6.5~10-5 mol/L cholesterol, a relative standard deviation was 1.5%. For the determinations of real sample, the addition standard recoveries were 95.0%- 105.0%, and the relative standard deviations were below 3.6%. The method has been applied to determine cholesterol in hogwash oil with satisfactory results.

关 键 词：化学发光 流动注射 地沟油 胆固醇 

分 类 号：O657.3[理学—分析化学]