气相色谱法测定食品中有机氯农药混合物的残留浓度

E. V. Melikhova, V. Y. Solovyova
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引用次数: 0

摘要

研究目的。目的是优化气相色谱法测定艾氏剂、六氯苯、七氯、α-六氯环己烷、γ-六氯环己烷、二氯二苯基三氯甲烷、二氯二苯基二氯乙烷和二氯二苯基二氯乙烯这八种有机氯农药混合物的条件。在对有机氯农药进行色谱研究时,我们使用了岛津 GC-2010Plus 气相色谱仪(日本岛津公司),该仪器配备了自动平衡蒸汽样品分配器 NT200N、基于 63Ni 的电子捕获检测器和石英毛细管非极性色谱柱 "Chromatek "SPB-5(30 米,0.32 毫米,膜厚 0.5 微米,基于苯基(5%)和二甲基(95%)聚硅氧烷),工作温度范围为 60°C 320/340°C。色谱图由 LabSolutions GPC 应用程序处理。在实验数据的基础上,选择了气相色谱测定和分离八组分有机氯农药混合物的最佳条件,即:流动相流量分度值为 1:10,载气流速为 1.0 ml/min,两级温度可编程色谱柱模式为 160 至 240°C,升温速率为 5°C/min。评估了分析的计量学特性,并用高效液相色谱法验证了拟议技术的结果。结果表明,色谱结果具有良好的重现性,可以检测到 10-6 - 10-5 μg/cm3 级别的有机氯农药。费舍尔检验表明,所研究的 COPCs 色谱分析方法同样准确,采样人群的重现性没有明显差异。建议对真实物体样本进行萃取样品制备,计算得出的萃取率大于 84%,因此建议将该技术用于分析物的定量测定。采用添加法测定了饮用水和婴儿果泥(俄罗斯)样品中有机氯农药的气相色谱分析方法。在研究的食品样品中没有检测到超过标准的有机氯农药残留量。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Gas Chromatographic Determination of Residual Concentrations of a Mixture of Organochlorine Pesticides in Food Products
Purpose of research. The aim of the work is to optimize the conditions for gas chromatographic determination of a mixture of eight organochlorine pesticides: aldrin, hexachlorobenzene, heptachlor, α-hexachlorocyclohexane, γ-hexachlorocyclohexane, dichlorodiphenyltrichloromethylmethane, dichlorodiphenyldichloroethane and dichlorodiphenyldichloroethylene.Methods. For chromatographic studies of organochlorine pesticides we used a Shimadzu GC-2010Plus gas chromatograph (Shimadzu, Japan) equipped with an automatic equilibrium vapor sample dispenser NT200N, electron-capture detector based on 63Ni and quartz capillary nonpolar column "Chromatek" SPB-5 (30 m, 0.32 mm, film thickness on the basis of phenyl(5%) and dimethyl(95%) polysiloxanes 0.5 μm) with an operating temperature range of 60°C 320/340°C. The chromatograms were processed in the application LabSolutions GPC.Results. On the basis of experimentally obtained data the optimal conditions for gas chromatographic determination and separation of eight-component mixture of organochlorine pesticides were selected, namely: the value of mobile phase flow division 1:10, carrier gas flow rate – 1.0 ml/min, two-stage temperature programmable column mode from 160 to 240°C with the rate of increase of 5°C/min. The metrological characteristics of the analysis and validation of the results of the proposed technique with the method of high-performance liquid chromatography were evaluated. Good reproducibility of chromatography results with the possibility of detection of organochlorine pesticides at the level of 10-6 – 10-5 μg/cm3 was proved. Application of Fisher's test has shown absence of significant differences in reproducibility of sampled populations the investigated methods of chromatographic analysis of COPCs are equally accurate. Extraction sample preparation of samples of real objects was proposed, the calculated extraction degrees >84% allow to recommend the technique for quantitative determination of analytes.Conclusion. The method of gas chromatographic analysis was tested for determination of organochlorine pesticides in samples of drinking water and baby puree (Russia) by additive method. Exceeding the norms of residual contents of organochlorine pesticides in the samples of the food products under study was not detected.
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