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采用加压液体萃取结合气相色谱串联质谱法测定以牛奶为基础的婴儿配方奶粉中的农药残留。

Determination of pesticides in milk-based infant formulas by pressurized liquid extraction followed by gas chromatography tandem mass spectrometry.

作者信息

Mezcua M, Repetti M R, Agüera A, Ferrer C, García-Reyes J F, Fernández-Alba A R

机构信息

Pesticide Residue Research Group, University of Almería, 04120 Almería, Spain.

出版信息

Anal Bioanal Chem. 2007 Nov;389(6):1833-40. doi: 10.1007/s00216-007-1501-y. Epub 2007 Aug 7.

Abstract

An efficient and selective automated analytical method for the determination and quantification of a selected group of 12 organochlorine and organophosphorous pesticides in milk-based infant formulas has been developed. The samples were extracted by pressurized liquid extraction (PLE) and analysed using GC-MS/MS. The use of alumina as the fat retainer in the PLE extraction cell, together with the application of an injector temperature program during the GC injection process, avoided typical matrix interferences without the application of additional cleanup steps. Mean recoveries of between 70 and 110% were achieved for most of the compounds, except for chlorpyrifos methyl (50%), vinclozoline (48%), fenitrothion (56%) and procymidone (53%), with relative standard deviations ranging from 9 to 17%. Low limits of quantification were obtained for the studied compounds, from 0.01 to 2.6 microg kg(-1), thus guaranteeing their accurate determination within the rigorous requirements established for baby food. The validated method was applied to a pilot monitoring study in Spain. Twenty five samples of different brands of powdered infant formulas were obtained from supermarkets. Positive findings of endosulfan I, endosulfan II, fenitrothion, chlorpyrifos ethyl and bifenthrin were detected at concentrations ranging from 0.03 to 5.03 microg kg(-1).

摘要

已开发出一种高效、选择性的自动化分析方法,用于测定和定量分析以牛奶为基础的婴儿配方奶粉中选定的一组12种有机氯和有机磷农药。样品通过加压液体萃取(PLE)进行萃取,并使用气相色谱-串联质谱(GC-MS/MS)进行分析。在PLE萃取池中使用氧化铝作为脂肪保留剂,以及在GC进样过程中应用进样器温度程序,无需额外的净化步骤即可避免典型的基质干扰。除甲基毒死蜱(50%)、乙烯菌核利(48%)、杀螟硫磷(56%)和腐霉利(53%)外,大多数化合物的平均回收率在70%至110%之间,相对标准偏差在9%至17%之间。所研究化合物的定量下限较低,为0.01至2.6微克/千克(-1),从而确保在为婴儿食品制定的严格要求范围内准确测定它们。该验证方法应用于西班牙的一项试点监测研究。从超市获取了25个不同品牌的婴儿配方奶粉粉末样品。检测到硫丹I、硫丹II、杀螟硫磷、乙基毒死蜱和联苯菊酯的阳性结果,浓度范围为0.03至5.03微克/千克(-1)。

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