摘要
番茄制品经乙腈提取,盐析,氟罗里硅土固相萃取小柱净化,微池电子捕获检测器(μECD)负化学源质谱(NCIMS)并联对净化液进行检测,一次进样可对番茄制品中的9种拟除虫菊酯类农药残留准确定量和确证。μECD回收率为87.6%～107.0%;相对标准偏差为5.5%～11.3%;检出限为0.0005～0.005mg/kg;负化学源选择离子(NCISIM)模式回收率为91.9%～109.7%;相对标准偏差为5.2%～12.7%;检出限为0.0005～0.005mg/kg(氯菊酯除外),两者之间没有显著的差别。该法快速、灵敏、准确,各项技术指标均满足农药残留检测的要求。
The product of processed tomato products sample extracted with acetonitrile was treated by a salting-out step, and purified by Florisil solid-phase extraction (SPE) cartridge. The final extract was injected (1 mu L) into a negative chemical ionization mass spectrometric (NCI/MS) system with micro-electron capture detector (mu ECD) for simultaneous analysis of the pyrethroids pesticide residues. Accurate quantitation and confirmation of nine pyrethroids pesticide residues was gained by one injection. When the spike level were 0.050 similar to 0.500 mg/kg, the recoveries for mu ECD ranged from 87.6% to 107.0% with the relative standard deviation of 5.5% to 11.3%, respectrity, the recoveries for negative chemical ionization/selected ion monitoring (NCI-SIM) mode ranged from 91.9% to 109.7% with the relative standard deviation of 5.2% to 12.7%. Limit, of detection (LOD) was 0.0005 similar to 0.005 mg/kg for mu ECD and 0.0005 similar to 0.005 mg/kg ( except permethrin) for NCI-SIM. There is no significant variation between the determination results of mu ECD and NCI-SIM. The method is rapid, sensitive and suitable for the analysis of pesticide residue.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2005年第6期838-842,共5页
Chinese Journal of Analytical Chemistry
