GC Determination of 22 Organochlorine Pesticides in Olive Oil
摘 要
橄榄油样品用乙腈提取,提取液用氮气浓缩至近干,残留物用正己烷稀释,采用硫酸磺化净化。采用气相色谱法测定样品溶液中22种有机氯农药的含量,22种有机氯农药采用Inert Cap 17色谱柱(30 m×0.25 mm,0.25 μm)分离,电子捕获检测器测定。22种有机氯农药的质量浓度在一定范围内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.001~0.01 mg·kg-1。以空白样品为基体进行加标回收试验,所得回收率为70.8%~120%,测定值的相对标准偏差(n=6)为0.40%~16%。
Abstract
Olive oil sample was extracted with acetonitrile, and then the extract was evaporated to near dryness by N2-blowing.The residue was diluted with n-hexane,and purified by sulfuric acid for sulphonation. GC was applied to the determination of 22 organochlorine pesticides in the sample solution. The 22 organochlorine pesticides were separated on Inert Cap 17 chromatographic column (30 m×0.25 mm, 0.25 μm) and detected by ECD. Linear relationships between values of peak area and mass concentration of the 22 organochlorine pesticides were kept in definite ranges. Detection limits (3S/N) of the method ranged from 0.001 to 0.01 mg·kg-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 70.8%-120%, with RSDs (n=6) of determined values in the range of 0.40%-16%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202005021
所属栏目 专题报道(药物分析)
基金项目
收稿日期 2019/9/25
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备注刘纲勇,博士,主要从事化妆品研究开发、原料检测工作
引用该论文: LIU Gangyong,HUANG Jinbo. GC Determination of 22 Organochlorine Pesticides in Olive Oil[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(5): 606~611
刘纲勇,黄锦波. 气相色谱法测定橄榄油中22种有机氯农药[J]. 理化检验-化学分册, 2020, 56(5): 606~611
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参考文献
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【3】毛敏明,周亮,肖有玉,等.农产品中常用农药残留快速检测方法概况[J].轻工标准与质量, 2017(4):26-29.
【4】徐娜.气相色谱法测定蔬果中的农药残留[J].农家参谋, 2018(3):47-47.
【5】范磊,黄素华,何日安,等.气相色谱-三重四极杆质谱法测定水中持久性有机氯污染物[J].中国环境监测, 2013,29(6):139-143.
【6】张辉.液相色谱法检测粮油农残的研究进展[J].食品工业, 2014,35(4):201-203.
【7】廖雅桦,庹苏行,钟科军,等.液质联用法在烟草农药残留检测方面的研究进展[J].广西轻工业, 2009,25(2):22-23.
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【10】张华,刘志广.仪器分析简明教程[M].大连:大连理工大学出版社, 2007.
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