Multiresidue analysis of organochlorine and pyrethroid pesticides in ground beef meat by gas chromatography-mass spectrometry
Multiresidue analysis of organochlorine and pyrethroid pesticides in ground beef meat by gas chromatography-mass spectrometry
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DOI：
10.1080/03601230902801000
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发表时间：
2009-01-01
影响因子：
2
通讯作者：
Dommarco, Roberto
中科院分区：
文献类型：
--
作者：
Stefanelli, Patrizia;Santilio, Angela;Dommarco, Roberto
建立并优化了牛肉样品中有机氯农药（OCPs）和拟除虫菊酯（PYRs）的多残留鉴别定量方法。样品提取由自动溶剂萃取器进行，萃取物由Extrelut NT3、Sep-Pack C18和florisil微型萃取盒组成的串联萃取盒系统进行清洗。最后采用气相色谱-四极杆质谱法（GC/MS）进行分析。从线性度、准确度、精密度、检出限（LOD）和定量限（LOQ）等方面考察了方法的性能。线性关系良好，相关系数(r2) > 0.98。除极易挥发的六氯苯（HCB）外，所调查的ocp和pyr的平均回收率分别为70- 110%和84- 99%。RSD%的范围从2%到15%。两类化合物的LOQ值均在0.005 ~ 0.1 mg/kg之间。所开发的方法已成功地对来自罗马（意大利）市场地区的50个商业牛肉样品进行了测试，证明是用于监测目的的常规多残留分析ocp和pyr的有用工具。所有感兴趣的化合物均未超过其各自的定量限。
A multiresidue method was developed and optimized for the identification/quantification of organochlorine pesticides (OCPs) and pyrethroids (PYRs) in beef meat samples. Samples extraction was performed by an automated solvent extractor and the extracts were cleaned-up by a tandem-cartridge system consisting of an Extrelut NT3 combined with a Sep-Pack C18 cartridge and a florisil minicartridge. Analysis was finally carried out by gas chromatography coupled with quadrupole mass spectrometry (GC/MS). The performance of the method was investigated in terms of linearity, accuracy, precision, detection limit (LOD) and quantification limit (LOQ). Good linearity was obtained, with correlation coefficients (r2) higher than 0.98. Mean recoveries were found in the ranges 70-110 % and 84-99 % for the investigated OCPs and PYRs, respectively, with the exception of extremely volatile hexachlorobenzene (HCB). RSD% turned out to range from 2 to 15 %. LOQ values were in the range 0.005-0.1 mg/kg for either class of compounds. The method developed was successfully tested on 50 commercial beef meat samples from the market area of Rome (Italy), proving to be a useful tool in routine multiresidue analysis of OCPs and PYRs for monitoring purposes. None of the compounds of interest were observed above their respective LOQ.