摘要
目的建立测定18种中药材及饮片中有机磷和氨基甲酸酯类农药残留量的GC-MS方法。方法样品经乙腈-丙酮超声提取,经无水硫酸钠-硅镁型吸附剂-无水硫酸钠色谱柱净化,用GC-MS法测定18种中药材及饮片中有机磷和氨基甲酸酯类农药的残留量。结果有机磷和氨基甲酸酯类农药残留量测定的线性范围为0.8~3.2ng,相关系数r≥0.990,平均回收率为56.2%~118.5%,重复性RSD值为0.2%~11.2%,稳定性RSD值小于3%。其中敌敌畏、仲丁威、二嗪农、抗蚜威和马拉硫磷在107批药材中的含量均小于0.15mg·kg-1。结论该方法灵敏度高,净化效果好,符合农药残留的检测要求。
Objective To establish a GC-MS method for the determination of organophsphate and carbamate pesticide residues in 18 kinds of Chinese herbal medicines.Methods The samples were extracted with acetonitrile-acetone and ultrasonic vibrations,and the samples were purified by anhydrous sodium sulfate-Florisil-anhydrous sodium sulfate.The contents of organophosphate and carbamate pesticides residues in 18 kinds of Chinese herbal medicines and herbal pieces were measured by GC-MS.Results Linear relationship for organophosphate and carbamate pesticides residues was measured in 0.8-3.2ng,the correlation coefficient r≥0.990,the average recoveries were 56.2%-118.5%,the RSD of repeatability was 0.2%-11.2%,the RSD of stability was less than 3%.Only dichlorvos,bassa,diazinon,pirimicarb and malathion in 107 batches of Chinese herbal medicines were less than 0.15mg·kg-1.Conclusion This method is sensitive with good purifying effect,and in line with pesticide residue testing standards.
出处
《西北药学杂志》
CAS
2017年第1期9-13,共5页
Northwest Pharmaceutical Journal
基金
"十二五"国家"重大新药创制"专项(编号:2014ZX09304307)
