GC-MS Determination of Residual Amounts of 22 Pesticides in Textiles
摘 要
提出了气相色谱-质谱法测定纺织品中22种农药残留量的方法。样品以正己烷-丙酮(1+1)混合溶液为提取剂,经加速溶剂萃取仪提取后,在40 ℃旋转蒸发仪中浓缩、氮气吹干后,用正己烷-丙酮(1+1)混合溶液溶解定容至2.0 mL,通过Agilent HP-5MS石英毛细管色谱柱(30 m×0.25 mm,0.25 μm)分离,采用电子轰击离子源选择离子监测模式进行质谱测定。22种农药的检出限(3S/N)在0.003~0.03 mg·kg-1之间。以空白棉布样品为基体,加入标准溶液进行回收试验,测得回收率在80.1%~95.9%之间,相对标准偏差(n=6)均小于13%。
Abstract
GC-MS was applied to the determination of residual amounts of 22 pesticides in textiles. The sample was extracted with a mixture of n-hexane-acetone (1+1) by accelerated solvent extraction, and the extract was concentrated in a rotary evaporator at 40 ℃ and evaporated to dryness by N2-blowing. The residue obtained was dissolved and made up to 2.0 mL with n-hexane-acetone (1+1) solution, which was used for GC-MS analysis. The Agilent HP-5MS (30 m×0.25 mm, 0.25 μm) capillary chromatographic column was used for separation, and the electron impact ionization source with selected ion monitoring (SIM) was adopted in MS. Values of detection limit of 22 pesticides found were in the range of 0.003-0.03 mg·kg-1. On the base of blank sample of cotton fabric, test for recovery was made by standard addition method, values of recovery found were in the range of 80.1%-95.9%, with RSD′s (n=6) less than 13%.
中图分类号 O657.7
所属栏目 工作简报
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收稿日期 2011/9/6
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备注柳彩云(1982-),女,黑龙江虎林人,硕士,主要从事分析化学工作。
引用该论文: LIU Cai-yun,MA Wei,CHEN Wei,LI Xiang,ZHONG Wei-ke,YU Jing,WANG Xiu-jun. GC-MS Determination of Residual Amounts of 22 Pesticides in Textiles[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(11): 1303~1306
柳彩云,马微,陈伟,李翔,仲维科,于静,王秀君. 气相色谱-质谱法测定纺织品中22种农药残留[J]. 理化检验-化学分册, 2012, 48(11): 1303~1306
被引情况:
【1】冯伟,张代辉,张勋,杨璐,赵韫慧,滕国生, "QuEChERS法提取-气相色谱-串联质谱法测定生态纺织品中31种农药残留",理化检验-化学分册 51, 1386-1392(2015)
【2】曹艳平,杨路平,邵立君, "气相色谱-质谱法测定茶叶中23种农药残留量",理化检验-化学分册 51, 647-650(2015)
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参考文献
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【3】申中兰,蔡继宝,高芸,等.基质固相分散-加速溶剂萃取-气相色谱法测土壤中有机氯农药残留[J].分析化学, 2005,33(9):1318-1320.
【4】吴刚,鲍晓霞,王华雄,等.加速溶剂萃取-凝胶渗透色谱净化-气相色谱快速分析动物源性食品中残留的多种有机磷农药[J].色谱, 2008,26(5):577-582.
【5】胡贝贞,宋伟华,谢丽萍,等.加速溶剂萃取/凝胶渗透色谱-固相萃取净化/气相色谱-质谱法测定茶叶中残留的33种农药[J].色谱, 2008,26(1):22-28.
【6】李冬梅.利用加速溶剂萃取仪测定食品中有机磷农药残留方法探讨[J].首都公共卫生, 2007,1(5):235-236.
【7】王淑红,熊英,王祥红.加速溶剂萃取法用于灯盏细辛中灯盏乙素的测定[J].药物分析杂志, 2006,26(5):703-705.
【8】陈军辉,杨佰娟,李文龙,等.加速溶剂萃取技术在中药有效成分分析中的应用[J].色谱, 2007,25(5):628-632.
【9】王明泰,靳颖,牟峻,等.GC-MS法测定纺织品中77种农药残留量[J].印染, 2007,33(4):37-41.
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