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膜固相萃取-气相色谱法测定饮用水中有机氯农药的技术优化与质量控制研究

Study on technical optimization and quality control of determination of organochlorine pesticides in drinking water by disk solid phase extraction-gas chromatography

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【作者】 韩志宇; 詹未; 张永; 李勇; 李浩然; 陶晶;

【Author】 HAN Zhiyu;ZHAN Wei;ZHANG Yong;LI Yong;LI Haoran;TAO Jing;Institute for Environmental Health,Beijing Center for Disease Prevention and Control;

【通讯作者】 陶晶;

【机构】 北京市疾病预防控制中心环境卫生所;

【摘要】 目的 建立膜固相萃取-气相色谱法测定饮用水中有机氯农药六氯苯、α-六六六、γ-六六六、七氯、β-六六六、δ-六六六、p,p’-DDE、o,p’-DDT、p,p’-DDD、p,p’-DDT的方法,以加标回收-质控图进行评估,保证检测的质量水平。方法 采用47 mm的C18固相萃取膜富集1 L饮用水样品,以二氯甲烷和乙酸乙酯洗脱后浓缩至1 m L。采用VF-1701ms型色谱柱,程序升温分离六氯苯、α-六六六、γ-六六六、七氯、β-六六六、δ-六六六、p,p’-DDE、o,p’-DDT、p,p’-DDD、p,p’-DDT,经电子捕获检测器测定,外标法定量。结果 10种有机氯农药标准于10~100μg/L范围内线性良好,相关系数>0.998 8,方法检出限为3~5 ng/L,低、中、高浓度平均加标回收率为87.7%~116.0%,相对标准偏差为8.3%~15.4%。加标回收质量控制图(n=20)中心线为91.8%~115.3%,标准偏差(s)为11.5%~14.1%。结论 本研究应用于饮用水监测具有高度的普及性,便捷高效,加标回收-质控图可有效控制检测的质量水平。

【Abstract】 Objective To establish a method for the determination oforganochlorine pesticides,including hexachlorobenzene,α-HCH,γ-HCH,heptachlor,β-HCH,δ-HCH,p,p’-DDE,o,p’-DDT,p,p’-DDD and p,p’-DDT,by using disk solid phase extractiongas chromatography,evaluate with recovery rate-quality control chart to ensure the quality level of testing. Methods 1 L drinking water sample was enriched by using a 47 mm C18 solid-phase extraction membrane,and methylene chloride and ethyl acetate were used for elution,and the constant volume was 1 mL. The hexachlorobenzene,α-HCH,γ-HCH,heptachlor,β-HCH,δ-HCH,p,p’-DDE,o,p’-DDT,p,p’-DDD and p,p’-DDT were separated by temperature programming with chromatographic column VF-1701 ms,and electron capture detector was used to collect data. The quantitation was carried out by the external standard method.Results 10 kinds of organochlorine pesticides showed the good linearity in 10-100 μg/L,and the correlation coefficientswere>0.998 8. The limits of detectionwere 3-5 ng/L. The average recoveries ranged from 87.7% to 116.0% for low,medium,and high concentrations,and the relative standard deviations were 8.3%-15.4%. The center lines of recovery rate-quality control chart(n=20)ranged from 91.8% to 115.3%,and standard deviations(s) were in the range of 11.5%-14.1%. Conclusion This method is simple,quick,and widely used in drinking water monitoring,and the recovery rate-quality control chart can improve the quality of inspection.

  • 【文献出处】 职业与健康 ,Occupation and Health , 编辑部邮箱 ,2023年19期
  • 【分类号】O657.71;TU991.21
  • 【下载频次】11
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