【求助】－有谁做过大蒜的农残检测的？

chlorpyrifos
cypermethrin
fenvalerate

青岛商检已经十分成功解决了你提出的问题。方法是将大蒜去皮后（整瓣，不要切片）放入微波炉中中火40秒钟。然后用PSA柱进行SPE萃取，干扰物很少。具体方法没有带在身边。如果你需要可以直接联系我。

chen_xh888@163.net

如果要检测六六六和DDT怎么净化啊？

提取之后直接用浓硫酸磺化即可。

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[url=https://insevent.instrument.com.cn/t/Mp]气相色谱法检测大蒜中二甲戊灵的残留量[/url]

Determination of Herbicide Residues in Garlic by GC–MS
Zilei Chen, Hong Zhang, Bing Liu, et al.
Chromatographia, Volume 66, Numbers 11-12, 2007, 887-891
Abstract：
A rapid multi-residue method has been developed for the determination of 16 herbicides in garlic. The analytical procedure is based on prior microwave heating prevention of the generation of sulfur-containing compounds. The garlic samples which had been pretreated were extracted with acetonitrile and cleaned up by solid-phase extraction. The herbicide residues were detected by gas chromatography–mass spectrometry with selected ion monitoring. The recoveries of 16 herbicides ranged from 69.0 to 105.4% with the relative standard deviations (RSD) below 10.1%. The limit of quantification (LOQ) ranged from 0.003 to 0.015 mg kg−1.

Supercritical fluid extraction and off-line clean-up for the analysis of organochlorine pesticide residues in garlic
Jian Hua Wanga, Qiang Xua,Kui Jiao
Journal of Chromatography A; Volume 818, Issue 1, 28 August 1998, Pages 138-143
Abstract
An approach using supercritical fluid extraction (SFE) followed by clean-up with a AgNO3-loaded Florisil column was utilized for the analysis of four organochlorine pesticides (OCPs) in garlic. The organic sulfur extracted by SFE from garlic was removed by AgNO3 allowing OCPs to be determined by GC–electron-capture detection without interferences. All OCPs recoveries ranged from 85.0% to 110.0% and relative standard deviations were in the range of 3.9–7.2% for spiked samples. The described method may be used to analyze OCPs in garlic on a routine basis.