固相萃取-气质联用法测定食用菌与生姜中的多组分农药残留
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秦国富 男 检验师 研究方向为食品卫生检验 E-mail:qinguofu123@126.com通讯作者:┣┣(中)通信作者┫┫李永波 女 高级工程师 研究方向为食品安全监测和药物分析 E-mail:lyb981238@163.com

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Determination of multiple pesticide residues in mushroom and ginger by SPE-GC/MS
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    摘要:

    建立一种固相萃取-气相色谱质谱联用法测定食用菌与生姜中的49种农药残留的方法,并对74份食用菌和22份生姜进行了分析测定。方法 鲜食用菌和生姜用乙腈提取,干食用菌用丙酮提取,提取液浓缩后采用固相萃取拄净化,DB-1701毛细管柱(30m×0.25mm×0.25μm)对农药进行分离,GC/MS检测进样口温度250℃,载气为氦气,恒流1.0ml/min,不分流进样,进样1μl;离子监测扫描(SIM)离子源温度230℃,接口温度280℃,电子能量70eV,溶剂延迟4min.。结果 49种农药在0.25~2.00μg/ml质量浓度范围内呈良好的线性关系,相关系数(r)为0.9890~0.9997,在8和80μg/kg两个浓度水平的加标回收率为66.5%~143.8%,RSD为2.2%~10.8%,检出限为0.1~10.0μg/kg。结论 本方法简单、快速、可靠,能够满足鲜食用菌与生姜中49种农药残留量的检测分析要求。

    Abstract:

    A method for determination of 49pesticide residues in mushroom and ginger by SPE-GC/MS was established, and 74mushroom and 22ginger samples were detected.MethodsThe pesticide residues in fresh mushroom and ginger were extracted with acetonitrile, and dry mushroom was extracted with acetone. The extracts were purified by SPE after being concentrated, and DB-1701capillary column was used for separation. ResultsThere was a good linearity between the peak area and the concentration of 49pesticide residues within 0.25μg/ml-2μg/ml, the correlation coefficients were 0.9890-0.9997, the recoveries of spiked sample at 8and 80μg/kg to fresh mushroom and ginger were ranged from 66.5%-143.8%, RSDs were ranged from 2.2%-10.8%, and the detection limits were ranged from 0.1-10.0μg/kg. ConclusionThe method was simple, rapid and reliable. It could be applied to determine pesticide residues in fresh mushroom and ginger.

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秦国富,李永波,李红光.固相萃取-气质联用法测定食用菌与生姜中的多组分农药残留[J].中国食品卫生杂志,2013,25(6):528-532.

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  • 收稿日期:2013-08-29
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  • 在线发布日期: 2013-12-31
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