建立了气相色谱-质谱联用(GC-MS)同时测定二甲戊灵和乙氧氟草醚在生姜、茎秆和土壤中残留量的分析方法,并采用该方法研究了两种农药在土壤中的消解动态及在土壤和生姜中的最终残留。样品前处理采用Qu ECh ERS法,经乙腈提取,姜块和茎秆提取液分别用N-丙基乙二胺(PSA)和石墨化碳黑(GCB)净化,土壤提取液用弗罗里硅土柱净化,选择离子监测模式(SIM)扫描,外标峰面积法定量。结果表明:当添加水平为0.01~0.5 mg/kg时,二甲戊灵在生姜、茎秆和土壤中的回收率分别为91%~100%、90%~98%和86%~100%,相对标准偏差(RSD)分别为3.2%~3.7%、2.7%~4.2%和3.2%~5.1%;乙氧氟草醚在生姜、茎秆和土壤中的回收率分别为90%~95%、86%~91%和85%~95%,RSD分别为2.4%~4.4%、3.9%~5.5%和2.3%~4.9%;样品中二甲戊灵和乙氧氟草醚的定量限(LOQ)均为0.01 mg/kg。二甲戊灵在土壤中的消解半衰期在12.5~20.5 d之间,乙氧氟草醚在18.8~25.6 d之间。采用33%二甲戊灵乳油和24%乙氧氟草醚乳油混剂分别按推荐剂量(有效成分693 g/hm~2和72 g/hm~2)和高剂量(有效成分1 039 g/hm~2和108 g/hm~2)于种植后施药1次,在生姜收获期的姜块中均未检出二甲戊灵和乙氧氟草醚残留。研究结果可为二甲戊灵和乙氧氟草醚在生姜上的合理使用及其最大允许残留限量(MRL)标准制定提供参考。
An analytical method was developed for the determination of pendimethalin and oxyfluorfen in Zingiber officinale Roscoe(ginger), Z. officinale stem and soil using gas chromatography-tandem mass spectrometry(GC-MS). The final residues of the above two herbicides in Z. officinale and their dissipation dynamics in soil were studied using this new method. A simple and efficient pretreatment method called Qu ECh ERS was used and samples were extracted with acetonitrile. Primary-secondary amine(PSA) and graphitized carbon black(GCB) were used to purify the Z. officinale and stem samples and Florisil was used to purify the soil samples.Ion scanning module(SIM) was selected for the mass spectrometry determination and the external standard and peak area method is employed for quantitative analysis. At the spiked levels of 0.01-0.5 mg/kg, the average recoveries of pendimethalin in Z.officinale, stem and soil were 91%-100%, 90%-98% and 86%-100%, respectively, and the relative standard deviations were 3.2%-3.7%, 2.7-4.2% and 3.2%-5.1%, respectively; the average recoveries of oxyfluorfen in Z. officinale, stem and soil were 90%-95%, 86%-91% and 85%-95%, respectively, and the relative standard deviations were 2.4%-4.4%, 3.9%-5.5% and 2.3%-4.9%, respectively, the limit of quantity(LOQ) of pendimethalin and oxyfluorfen samples were both 0.01 mg/kg. The dissipation halflives of pendimethalin in soil were 12.5-20.5 days and the dissipation half-lives of oxyfluorfen in soil were 18.8-25.6 days in the ginger field study. When 33% pendimethalin emul-sifiable concentrate(EC)and 24% oxyfluorfen EC were sprayed at the recommended dose(active ingredients: 693 g/hm^2 and 72 g/hm^2) and high dose(active ingredients: 1 039 g/hm^2 and 108 g/hm^2) once after Z. officinale was planted, the pendimethalin and oxyfluorfen residues were not detected in Z. officinale in the harvest period. The results can provide a reference for the rational use and the maximum residue limits(MRL) standard development of