气相色谱-质谱联用检测农药制剂中8种有机溶剂类助剂的含量及市场样品筛查
投稿时间:2018-08-17      点此下载全文 HTML
引用本文:林琴,周利,张新忠,等.气相色谱-质谱联用检测农药制剂中8种有机溶剂类助剂的含量及市场样品筛查[J].农药学学报,2019,21(1):119-124.
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作者单位E-mail
林琴 中国农业科学院 茶叶研究所, 杭州 310008  
周利 中国农业科学院 茶叶研究所, 杭州 310008  
张新忠 中国农业科学院 茶叶研究所, 杭州 310008  
楼正云 中国农业科学院 茶叶研究所, 杭州 310008  
罗逢健 中国农业科学院 茶叶研究所, 杭州 310008 lfj@tricaas.com 
陈宗懋 中国农业科学院 茶叶研究所, 杭州 310008 zmchen2006@163.com 
基金项目:科技基础性工作专项(2013FY110100-2);浙江省自然科学基金(LY18C16005);国家重点研发计划(2016YFD0200207-2);中国农业科学院创新工程(CAAS-ASTIP-TRICAAS)
中文摘要:建立了农药制剂中甲醇、甲苯、乙苯、邻二甲苯、对二甲苯、间二甲苯、N,N-二甲基甲酰胺(DMF)和二甲基亚砜(DMSO)8种有机溶剂类助剂的气相色谱-质谱联用(GC-MS)测定方法,并运用该方法对市售的206种液体农药制剂进行了检测,获得市售农药制剂中目标助剂的含量。农药制剂经乙腈稀释10 000倍后,在选择离子监测(SIM)模式下测定,8种助剂的质量浓度与对应的峰面积间线性相关性良好,r为0.999 2~0.999 8;8种助剂在100~1 000 mg/kg添加水平下,回收率为76%~116%,相对标准偏差(RSD)均小于17%;8种助剂的定量限(LOQ)在100~500 mg/kg之间。对206种市售液体农药制剂的筛查结果表明:8种助剂的检出率在0.5%~31.1%之间,超标率在7.2%~14.5%之间,液体农药制剂中苯类溶剂使用量较高。该方法可为农药加工、管理和助剂限量标准制定提供依据,农药制剂中有毒溶剂的使用应引起生产企业和农药管理部门的重视。
中文关键词:农药制剂  助剂  有机溶剂  气相色谱-质谱联用  筛查  检出率
 
Analytical method and sample screening of eight organic solvent adjuvants in pesticide formulations using gas chromatography-mass spectrometry
Abstract:An analytical method was developed to simultaneously determine inert ingredients, such asmethanol, toluene, ethylbenzene, O-xylene, para-xylene, meta-xylene, N, N-dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) in pesticide formulations using gas chromatography-mass spectrometry. The method was applied to the detection of inert ingredients in 206 commercial liquid pesticide formulations. The pesticide formulations were diluted 10 000 times by acetonitrile, and the target inert ingredients were detected in selective ion monitor (SIM) mode. The linearity of 8 inert ingredients ranged from 0.999 2 to 0.999 8. The recoveries were between 76% to 116%, with the relative standard deviations (RSD) were lower than 17% at the spiked level of 100-1 000 mg/kg. The limits of quantitations (LOQ) were 100-500 mg/kg. The level of inert ingredients ranged from 0.5%-31.1% in 206 commercial liquid pesticide products. The content of inert ingredients in 7.2%-14.5% of the pesticide products were higher than the proposed maximum residue limits. High application rates of benzene organic solvents were detected in liquid pesticide formulations. This new method could supply reference for pesticide production, pesticide administration and fixation of maximum residue limits. Our results indicated that the usage of the harmful organic solvent in pesticides production was a noteworthy problem.
Key words:pesticide formulations  adjuvants  organic solvents  gas chromatography-mass spectrometry  screening  detection rate
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