【摘要】：基于溶劑提取-固相微萃取-氣質(zhì)聯(lián)用技術(shù)建立了新鮮肝臟中26種常見投毒農(nóng)藥的快速篩查與定量方法。通過考察有機(jī)溶劑、萃取頭、萃取溫度等影響因素優(yōu)化萃取條件;新鮮肝臟經(jīng)丙酮水溶液提取,離心分離、氮吹濃縮后補(bǔ)充超純水,經(jīng)SPME萃取后采用GC-MS進(jìn)行定性篩查與定量分析。實(shí)驗(yàn)結(jié)果表明,以丙酮水溶液(4:1,V/V)提取,選擇PDMS/DVB/CAR萃取頭,在pH 7.4緩沖溶液體系下、室溫下(20℃)萃取30 min,攪拌速度為200 r/min時(shí)萃取效率最高;新鮮肝臟中26種農(nóng)藥在50~200 ng/g范圍內(nèi)具有良好的線性,相關(guān)系數(shù)均≥0.992,方法檢出限(LOD)為0.15~16 ng/g(S/N=3),定量限(LOQ)為0.48~48 ng/g(S/N=10);在加入量為50,100,200 ng/g時(shí),農(nóng)藥混合標(biāo)準(zhǔn)溶液的回收率為66.7%~108.2%,相對(duì)標(biāo)準(zhǔn)偏差為1.4%~16%。方法適用于對(duì)投毒案件受害者肝臟中常見投毒農(nóng)藥進(jìn)行快速篩查與定量分析。
[Abstract]:A rapid screening and quantification method for 26 common toxic pesticides in fresh liver was established based on solvent extraction solid phase microextraction and GC-MS. The extraction conditions were optimized by investigating the influencing factors such as organic solvent, extraction head and extraction temperature. The fresh liver was extracted by acetone aqueous solution, centrifuged and concentrated by nitrogen, then supplemented with ultrapure water. GC-MS was used for qualitative screening and quantitative analysis after SPME extraction. The experimental results show that the PDMS/DVB/CAR extractor is extracted with acetone aqueous solution (4: 1 V / V) and extracted 30 min, at room temperature (20 鈩，

本文編號(hào)：2318201