摘要
采用程序升温大体积进样技术（PTV-LVI）及Qu ECh ERS方法建立了果汁中90种农药多残留的气相色谱-质谱分析方法。样品用乙腈提取,经Mg SO4和Na Cl除水后,以PSA和C18柱净化,用大体积进样技术的气相色谱-质谱进行测定。PTV-LVI优化参数为：初始温度100℃、分流出口吹扫流量50 m L/min、分流排空时间1.5 min、进样速度2μL/s。结果表明：90种农药在0.05~10μg/L的范围内呈良好线性关系,相关系数（R2）为0.9879~0.9999,相对标准偏差为3.4%~15.6%,平均回收率在70.3%~119.2%之间。90种农药的检出限均低于10μg/kg,定量限低于20μg/kg。本方法快速、简便、灵敏度高、重现性好,适用于果汁中的多种类农药残留分析。
A gas chromatography-mass spectrometric （GC-MS） method determination of 90 pesticide residues in fruit juices using programmab was established for the simultaneous le temperature vaporizer-based large volume injection （PTV-LVI） and QuEChERS Cleanup. The pesticides of fruits sample was extracted with acetonitrile, and after the water in the extractant was removed with anhydrous magnesium sulfate and sodium chloride, the pesticides were further cleaned up with dispersive method on PSA and C18, and detected by gas chromatography-tandem mass spectrometry under multiple reaction monitoring mode. Under the optimum PTV- LVI parameters including inlet temperature of 100℃, split vent flow rate at 50 mL/min, 1. 5 rain of evaporation time and 2μL/s of injection speed, GC-MS analysis for the pesticides was carried out. The results showed that, in the pesticides concentration range of 0. 05- 10 μg/L, the method kept good linear relationships with the correlative coefficients between 0.9879 and 0. 9999. The recoveries of the pesticide were from 70.3% to 119.2%, the relative standard deviations （RSDs） were between 3.4% and 15.6%. The limits of detection （LOD） were below 10μg/kg and the limit of Quantitation （LOQ） was less than 20 μg/kg. The method is simple, quick, safe, reproducible and applicable to confirm pesticide residue in the fruit juices samples.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2015年第8期1154-1161,共8页
Chinese Journal of Analytical Chemistry
基金
国际原子能机构技术援助项目(No.CPR5018)
"十一五"国家863计划(No.2006AA10Z449)
"十一五"国家科技支撑计划项目(Nos.2007BAD47B07
2009BADB7B04)
现代农业(柑桔)产业技术体系建设专项资助~~
关键词
果汁
农药多残留
大体积进样
气相色谱-质谱
QUECHERS
Fruit juices
Multi-residue pesticides
Large volume injection
Gas chromatography-massspectrometry
QuEChERS
