摘要
目的应用气相色谱-质谱联用方法(GC-MS)测定蔬菜样品中克百威、三羟基克百威及丁硫克百威的残留。方法使用不同pH值的缓冲溶液调节基质样品,经15 ml乙腈提取,漩涡振荡15 min后加入3 g氯化钠分层,剧烈振摇1 min取乙腈层,再重复一次,合并2次的乙腈层经固相萃取柱(Carb/NH2柱)净化提取浓缩后,供GC-MS测定。结果在浓度为0.5μg/ml^10.0μg/ml时相关系数均>0.99,将基质调节至pH=7.5,同时测定0.1 mg/kg和1.0 mg/kg的3种氨基甲酸酯的加标回收率为74.2%~120.7%,相对标准偏差为0.41%~2.63%。3种组分的检出限:克百威为0.01 mg/kg;三羟基克百威为0.02 mg/kg;丁硫克百威为0.01 mg/kg。结论通过对基质pH值的调节可以有效抑制部分克百威、三羟基克百威和丁硫克百威的降解及转化,抽检的20份蔬菜均检出克百威、三羟基克百威及丁硫克百威。
Objective To determine the residues of carbofuran, 3 - Hydroxycarbofuran and carbosulfan in vegetables by gas chromatography mass spectrometry （GC - MS）. Methods The sample which had been adjusted by pH buffer solutions was ex- tracted by 15 ml acetonitrile. After swirling shaving for 15 min, 3 g sodium chloride was added to separate acetonitrile layer with strongly shaking for 1 rain. The above operations were repeated, then the twice acetonitrile layers which had been merged togeth- er was purified by Carb/NH2 solid phase extraction column. Finally, the purified souhion was concentrated and analyzed by GC - MS. Results When the pH of substrate was adjusted to 7.5, the correlation coefficients could reach above 0.99 in the concentration range of 0.5 p^g/ml - 10.0 ~g/ml. The standard recovery rates of three components were within 74.2% - 120.7%, and the relative standard deviation was within 0.41% - 2.63%. The detection limits of the 3 compounds, carbofuran, 3 - Hydroxycarbofuran, and carbosulfan, were 0. 01 mg/kg, 0. 02 mg/kg and 0.01 mg/kg, respectively. Conclu- sion The method can suppress the degradation and conversion of carbofuran, 3 - Hydroxycarbofuran and carbosulfan through adjusting pH of substrate. There were no residues of carbofuran, 3 - Hydroxycarbofuran and carbosulfan detected randomly in the 20 vegetable samples.
出处
《中国卫生检验杂志》
CAS
2017年第11期1539-1541,共3页
Chinese Journal of Health Laboratory Technology
关键词
蔬菜
克百威
三羟基克百威
丁硫克百威
气质联用
Vegetables
Carbofuran
3 - Hydroxycarbofuran
Carbosulfan
Gas chromatography mass spectrometry
