SPE-GC/MS测定苹果梨中19种有机氯农药残留
作者:
作者单位:

(1. 延边朝鲜族自治州检验检测中心,吉林 延吉 133000; 2. 吉林烟草工业有限责任公司,吉林 延吉 133000; 3. 延边大学工学院,吉林 延吉 133002)

作者简介:

姚蕴恒,男,延边朝鲜族自治州检验检测中心工程师,硕士。

通讯作者:

任秀丽(1986—),女,延边大学讲师,硕士。E-mail: renxiuli@ybu.edu.cn

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基金项目:

国家市场监督管理总局科技计划项目(编号:S2019MK057)


Determination of 19 kinds of organchlorine pesticide residues in apple-pear by using gas chromatography-mass spectrometry coupled with solid-phase extraction
Author:
Affiliation:

(1. Inspection Center of Yanbian Korean Autonomous Prefecture, Yanji, Jilin 133000, China; 2. Jilin Tobacco Industry Co., Ltd., Yanji, Jilin 133000, China; 3. College of Engineering, Yanbian University, Yanji, Jilin 133002, China)

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    摘要:

    采用固相萃取技术结合气相色谱—质谱(SPE-GC/MS)技术建立了同时检测苹果梨中19种农药残留的分析方法,并对样品预处理过程中萃取剂、萃取剂用量、取样量、固相萃取柱、洗脱剂等条件进行优化,采用选择离子监测(SIM)模式,外标法定量。结果表明,19种农药在线性范围内线性关系良好(R2≥0.996 7);3个添加水平(20,40,200 μg/kg)的回收率为86.1%~108.9%,相对标准偏差<10%;19种农药检出限为3.0~6.0 μg/kg,定量限为10.0~20.0 μg/kg;该方法样品前处理简单、准确性好、灵敏度高,适用于苹果梨中19种农药残留的筛选与测定。

    Abstract:

    An analytical method for the simultaneous determination of 19 kinds of organochlorine pesticides in apple-pear was established based on optimized solid-phase extraction coupled with gas chromatography-mass spectrometry(SPE-GC/MS). Different extraction conditions, included extraction solvent, extraction solvent volume, sample weight, solid phase extraction clean-up and eluent were optimized during the sample pretreatment. The quantification were analyzed by GC/MS in selected ion monitoring (SIM) mode and the external standard method. The method showed good linearity (R2≥0.996 7) for all the pesticides. The recoveries at three spiked levels (20, 40, and 200 μg/kg) ranged from 86.1% to 108.9% with the relative standard deviation below 10%. The limit of detection ranged from 3 to 6 μg/kg and the limit of quantification ranged from 10.0 to 20.0 μg/kg the for 19 kinds of pesticides, respectively. The method was simple, accurate and showed high sensitivity for screening and detection of the 19 kinds of pesticides in apple-pear.

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姚蕴恒,白龙律,武伦鹏,等. SPE-GC/MS测定苹果梨中19种有机氯农药残留[J].食品与机械,2019,35(12):87-95.
YAO Yun heng, BAI Long lü, WU Lun peng, et al. Determination of 19 kinds of organchlorine pesticide residues in apple-pear by using gas chromatography-mass spectrometry coupled with solid-phase extraction[J]. Food & Machinery,2019,35(12):87-95.

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  • 收稿日期:2019-09-09
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  • 在线发布日期: 2022-10-05
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