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基于溶剂提取-固相微萃取-气质联用技术建立了新鲜肝脏中26种常见投毒农药的快速筛查与定量方法。通过考察有机溶剂、萃取头、萃取温度等影响因素优化萃取条件;新鲜肝脏经丙酮水溶液提取,离心分离、氮吹浓缩后补充超纯水,经SPME萃取后采用GC-MS进行定性筛查与定量分析。实验结果表明,以丙酮水溶液(4:1,V/V)提取,选择PDMS/DVB/CAR萃取头,在pH 7.4缓冲溶液体系下、室温下(20℃)萃取30 min,搅拌速度为200 r/min时萃取效率最高;新鲜肝脏中26种农药在50~200 ng/g范围内具有良好的线性,相关系数均≥0.992,方法检出限(LOD)为0.15~16 ng/g(S/N=3),定量限(LOQ)为0.48~48 ng/g(S/N=10);在加入量为50,100,200 ng/g时,农药混合标准溶液的回收率为66.7%~108.2%,相对标准偏差为1.4%~16%。方法适用于对投毒案件受害者肝脏中常见投毒农药进行快速筛查与定量分析。
A rapid screening and quantification method for 26 common pesticides in fresh liver was established based on solvent extraction-solid phase microextraction-gas chromatography-mass spectrometry. The extraction conditions of organic solvent, extraction head and extraction temperature were optimized. Fresh liver was extracted with acetone aqueous solution, centrifuged and concentrated by nitrogen. After ultrapure water was added, SPME was used for qualitative screening and quantitation by GC-MS analysis. The experimental results showed that PDMS / DVB / CAR extraction head was extracted with acetone aqueous solution (4: 1, V / V) and extracted at room temperature (20 ℃) for 30 min under pH 7.4 buffer solution. The stirring speed was 200 r The extraction efficiency of 26 pesticides in fresh liver ranged from 50 ng / g to 200 ng / g, the correlation coefficients were all ≥ 0.992, and the limit of detection (LOD) was 0.15-16 ng / g (S / The LOQ ranged from 0.48 to 48 ng / g (S / N = 10). The recoveries of pesticide mixed standard solutions were 66.7% -108.2% at 50,100 and 200 ng / g, The standard deviation is 1.4% ~ 16%. The method is suitable for rapid screening and quantitative analysis of commonly used pesticides in the liver of poisoned patients.