GC-MS Determination of Residual Amounts of 15 Phenoxy-Hydroxy-Acid Herbicides in Rice
摘 要
采用气相色谱-质谱法测定大米中15种苯氧羧酸类除草剂的残留量。优化的试验条件如下:1提取溶剂为乙腈;2衍生温度为30℃;3衍生时间为20 min;4净化萃取柱为Carbon TPT柱。在气相色谱分离中用PerkinElmer Elite-5MS毛细管柱为固定相,在质谱分析中采用全扫描和多反应监测模式。15种苯氧羧酸类除草剂的线性范围均为0.02~1.00 mg·L-1,方法的检出限(3S/N)为0.001~0.006 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80.3%~103%,测定值的相对标准偏差(n=5)为4.9%~9.8%。
Abstract
GC-MS was applied to the determination of residual amounts of 15 phenoxy-hydroxy-acid herbicides in rice. The optimized conditions found were as follows:1 extraction solvent was acetonitrile; 2 derivative temperature was 30℃; 3 derivative time was 20 min; 4 purified extraction column was Carbon TPT column. PerkinElmer Elite-5MS capillary column was used for GC separation. The full-scanning mode and the multiple reaction monitoring mode were adopted in MS determination. Linearity ranges of the 15 phenoxy-hydroxy-acid herbicides were found between 0.02 mg·L-1 and 1.00 mg·L-1 with detection limits (3S/N) in the range of 0.001-0.006 mg·kg-1. On the base of blank sample, test for recovery was made by standard addition method and values of recovery found were in the range of 80.3%-103%, with RSD's (n=5) in the range of 4.9%-9.8%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201711008
所属栏目 工作简报
基金项目 贵州省科技厅联合基金项目(TN2015-9);贵州省联合金[(2016)7374]
收稿日期 2016/11/19
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备注程寿峰(1983-),男,山东临沂人,讲师,研究方向为环境污染,chengfeng1218@126.com
引用该论文: CHENG Shoufeng,WEI Shaofeng,WANG Xingning,GOU Haichao,ZHANG Aihua. GC-MS Determination of Residual Amounts of 15 Phenoxy-Hydroxy-Acid Herbicides in Rice[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(11): 1281~1285
程寿峰,魏绍峰,王兴宁,苟海潮,张爱华. 气相色谱-质谱法测定大米中15种苯氧羧酸类除草剂的残留量[J]. 理化检验-化学分册, 2017, 53(11): 1281~1285
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