摘要
建立了气相色谱-电子捕获检测器(GC-ECD)测定中药材人参和西洋参中嘧菌酯残留的分析方法。样品经乙腈-水[V(乙腈)∶V(水)=7∶1]提取,柱层析[m(弗罗里硅土)∶m(中性氧化铝)∶m(活性炭)=5∶3∶0.15)及液-液分配净化,GC-ECD检测。结果表明,当嘧菌酯在人参和西洋参中的添加水平分别为1、0.5和0.01 mg/kg时,回收率分别为82.1%~97.8%和90.9%~92.0%,相对标准偏差(RSD)分别为1.6%~6.2%和1.6%~3.1%,均符合农药残留分析要求。仪器的最小检出量(LOD,S/N=3)为0.06 ng,方法的最低检测浓度(LOQ)为0.01 mg/kg。采用所建立方法调查了2010年不同来源人参和西洋参样品中嘧菌酯的残留情况,并对其膳食风险进行了初步评估。结果表明,样品中嘧菌酯的最大残留量为0.1 mg/kg,计算得出的风险商(RQ)值很小,处于安全水平。
A method for the determination of azoxystrobin residues in Panax ginseng and Panax quinquefolium was described.The residues were extracted with acetonitrile-water [V(acetonitrile):V(water) =7:1] assisted by ultrasonic,cleaned up with florisil-neutral alumina-activated charcoal(5:3:0.15,m:m:m) mixed column and dichloromethane by means of liquid-liquid partition.Quantitative analysis was performed with gas chromatography equipped with ECD(electronic capture detector).The fortified recoveries and relative standard deviation(RSD) were 82.1%-97.8% and 1.6%-6.2% in Panax ginseng,90.9%-92.0% and 1.6%-3.1% in Panax quinquefolium,at three spiked levels(1,0.5 and 0.01 mg/kg).The limit of detection(S/N=3) was 0.06 ng and the limit of quantification(LOQ) of the detection method was 0.01 mg/kg.The method was applied to monitor the residue status of azoxystrobin in some representative Panax ginseng and Panax quinquefolium planting areas and make risk assessment in 2010.The result of the study showed that the maximum residue in the sample was 0.1 mg/kg.By calculating,risk quotient(RQ) was very low and the residue could be declined to the safe level.
出处
《农药学学报》
CAS
CSCD
北大核心
2012年第1期67-73,共7页
Chinese Journal of Pesticide Science
基金
国家药典委员会国家标准提高研究课题
关键词
嘧菌酯
人参
西洋参
农药残留
风险评估
azoxystrobin
Panax ginseng
Panax quinquefolium
pesticide residue
risk assessment