气相色谱-质谱联用法测定水溶肥料中10种拟除虫菊酯类农药含量

Determination of 10 kinds of pyrethroid pesticides in water-soluble fertilizer by gas chromatography-mass spectrometry

中文关键词:  水溶肥料  拟除虫菊酯  气相色谱-质谱联用法

英文关键词:water soluble fertilizer  pyrethroid  gas chromatography-mass spectrometry

中文摘要:

      目的 建立气相色谱-质谱联用法测定肥料中10种拟除虫菊酯农药的分析方法。方法 样品经丙酮超声提取, DB-5MS毛细管气相色谱柱分离, 用气相色谱-质谱法测定。结果 10种化合物浓度在各自线性范围内与相应峰面积呈线性关系, 相关系数r＞0.990, 加标回收率为78.12%～120.63%, 精密度(relative standard deviation, RSD)为1.24%~11.91%。称样量为0.5 g时, 联苯菊酯检出限为0.06 mg/kg; 醚菊酯检出限为0.1 mg/kg; 甲氰菊酯、氯菊酯、氟胺氰菊酯检出限为0.2 mg/kg; 氯氟氰菊酯、氟氯氰菊酯、氯氰菊酯、氰戊菊酯、溴氰菊酯检出限为0.4 mg/kg。结论 该方法样品前处理简单、快捷, 重复性及回收率均能达到检测分析要求, 可以应用于水溶肥料中拟除虫菊酯农药的检测。

英文摘要:

      Objective To establish a method for the determination of 10 kinds of pyrethroid pesticides in water-soluble fertilizers by gas chromatography-mass spectrometry method. Methods The samples were ultrasonically extracted by acetone, separated by DB-5MS capillary gas chromatographic column and detected by GC-MS. Results There was a linear relationship between the mass concentration of the ten pyrethroid pesticides and the corresponding peak area, the correlation coefficient r>0.990. The recovery rate was 78.12%?120.63%, and the precision (RSD) was 1.24%?11.91%. When the sample amount was 0.5 g, the detection limit of bifenthrin was 0.06 mg/kg, etherinulin was 0.1 mg/kg; fenpropathrin, permethrin and flufenpropathrin was 0.2 mg/kg; cypermethrin, flufenpropathrin, cypermethrin, fenvalerate and deltamethrin method was 0.4 mg/kg. Conclusion The method is simple and fast, the repeatability and recovery can meet the requirement of detection and analysis. It can be applied to the detection of pyrethroid pesticides in water soluble fertilizer.