主题:【求助】玉米中农药残留分析资料

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kenneth06
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最近做玉米中农药残留,感觉很棘手,净化不好!
不知道那位高手有关于玉米中农药残留分析的外文资料啊,能否分享一下或则直接发给我(wwh0521@163.com)!我就查到一些中文的和一篇外文的资料!
另外如有做玉米中农药残留的经验,也希望各路大侠分享一下!
我做玉米中农药残留快一个月了,也没有找到快速、简便,能大批量处理样品的方法。GPC方法没有仪器!呵呵!
在此先谢谢啦!
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我在故我思
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Determination of 36 pesticide residues in corn using gas chromatography mass spectrometry

Liu Pengyan, Ma Yusong
(College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China)

Received  Sep. 26, 2004; Hebei Science and Technology Department, and Science and Technology Bureau, of Baoding city. (Project: 03547023D, 03N006)

Abstract:
A new analytical method has been developed to determine organophosphorus, organochlorine, carbamate and pyrethroid, multicomponent pesticide residues in corn. It is based on a fast extraction of pesticides with dichloromethane and a further clean-up procedure by solid-phase extraction using a Florisil cartridge, then analysed by gas chromatography-mass spectrometry (GC-MS). The pesticides were identified by retention time and the proportion of qualitative ions, and quantified being base on extract of spiking standards in blank sample. The determination results of accuracy, precision and the limits of detection (LOD) was shown that the method was validated.

Keywords: GC-MS, pesticides, multi-residues, corn

全文链接: http://china.chemistrymag.org/cji/2005/071013pe.htm
我在故我思
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楼主,下面有及几篇外文的文献,一篇是关于玉米中农药残留提取的,两篇是高脂肪含量样品中农残提取的:
Multi-Residue Analysis of Corn and Soybean Pesticides in Brazilian Oxisols Using Gas Chromatography and Mass Selective Detection
V. Laabs*, W. Amelung and W. Zech
Institute of Soil Science and Soil Geography, Univ. of Bayreuth, 95440 Bayreuth, Germany.

ABSTRACT:
Available methods for measuring pesticide residues in soils usually have not been tested for tropical soils nor do they cope with the spectrum of pesticides used in the tropics. An accurate and efficient method for the simultaneous determination of 14 corn (Zea mays L.) and soybean [Glycine max (L.) Merr.] pesticides in Oxisols is presented in this study. The quantification of the pesticides was achieved using gas chromatography coupled with mass selective detection. For the extraction of aged pesticide residues from soil samples, combinations of acetone, ethylacetate, hexane, methanol, water, and salt solutions were tested. Of the 20 different solvent systems evaluated, the mixture of acetone-ethylacetate-water 2:2:1 (v/v/v) was most efficient for the extraction of all pesticides except metribuzine [4-amino-6- (1,1-dimethylethyl)-3-(methylthio)-1,2,3- triazine-5(4H)-one]; this herbicide was recovered best by ethylacetate-water4:1 (v/v). Different sample aging-times (5–30d) did not affect the recovery of pesticides from incubated samples. Extraction of pesticides from field-soil samples also was best with acetone-ethylacetate-water. No differences in extraction efficiency were observed between a simple shake extraction (4h) and batch extractions with an additional rise in temperature (60°C) or a sonication (30 min). The elimination of the water from the soil extract was achieved by a liquid-liquid extraction with dichloromethane, which recovered the whole polarity spectrum of pesticides quantitatively. The method recovery from soil samples of freshly spiked pesticides averaged 94.8 ± 2.4%. The method was validated for Oxisols of contrasting clay and organic C content.

Pesticide residue analyses in plant material by chromatographic methods: clean-up procedures and selective detectors
Jozef Tekel′a,  and  tefan Hatríkb
Abstract:
This paper deals with the analysis of pesticide residues by chromatographic methods in samples of plant origin. Emphasis is put on the isolation and clean-up steps of the sample preparation for GG or $$lc determination. The problems of the extraction solvent selection and clean-up procedures using different types of adsorption column chromatography or gel permeation chromatography are discussed. Attention is also given to alternative techniques such as supercritical fluid extraction (SFE), matrix solid-phase dispersion (extraction) (MSPD) and sweep co-distillation that are used for sample processing prior to gc and $$lc analysis. Currently, pesticide residue analyses are typically multi-residue procedures with highly sensitive methods. Consumption of costly and toxic solvents is being minimized and fully automated analytical procedures can be expected in the future.
这篇是综述,里面应该有一些参考文献,您能参考的。


Evaluation of Two Fast and Easy Methods for Pesticide Residue Analysis in Fatty Food Matrixes
Author(s): Steven J. Lehotay 1 | Kateřina Maštovská 2 | Seon Jong Yun 3 

Abstract:
Two rapid methods of sample preparation and analysis of fatty foods (e.g., milk, eggs, and avocado) were evaluated and compared for 32 pesticide residues representing a wide range of physicochemical properties. One method, dubbed the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for pesticide residue analysis, entailed extraction of 15 g sample with 15 mL acetonitrile (MeCN) containing 1% acetic acid followed by addition of 6 g anhydrous magnesium sulfate and 1.5 g sodium acetate. After centrifugation, 1 mL of the buffered MeCN extract underwent a cleanup step (in a technique known as dispersive solid-phase extraction) using 50 mg each of C18 and primary secondary amine sorbents plus 150 mg MgSO4. The second method incorporated a form of matrix solid-phase dispersion (MSPD), in which 0.5 g sample plus 2 g C18 and 2 g anhydrous sodium sulfate was mixed in a mortar and pestle and added above a 2 g Florisil column on a vacuum manifold. Then, 5 × 2 mL MeCN was used to elute the pesticide analytes from the sample into a collection tube, and the extract was concentrated to 0.5 mL by evaporation. Extracts in both methods were analyzed concurrently by gas chromatography/mass spectrometry and liquid chromatography/tandem mass spectrometry. The recoveries of semi-polar and polar pesticides were typically 100% in both methods (except that basic pesticides, such as thiabendazole and imazalil, were not recovered in the MSPD method), but recovery of nonpolar pesticides decreased as fat content of the sample increased. This trend was more pronounced in the QuEChERS method, in which case the most lipophilic analyte tested, hexachlorobenzene, gave 27 ± 1% recovery (n = 6) in avocado (15% fat) with a <10 ng/g limit of quantitation.

很抱歉没有全文,我已经到到文献求助-应助版面发帖求助了:  http://www.instrument.com.cn/bbs/shtml/20080430/1243390/。




pingguwu
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原文由kenneth06发表:最近做玉米中农药残留,感觉很棘手,净化不好!不知道那位高手有关于玉米中农药残留分析的外文资料啊,能否分享一下或则直接发给我(wwh0521@163.com)!我就查到一些中文的和一篇外文的资料!另外如有做玉米中农药残留的经验,也希望各路大侠分享一下!我做玉米中农药残留快一个月了,也没有找到快速、简便,能大批量处理样品的方法。GPC方法没有仪器!

  做农药分析,首先看看自己实验室条件,确定仪器检测方法,然后确定要分析的农药品种,有的时候反过来,先确定项目再找仪器,最后进行样品前处理攻关,玉米主要干扰物是色素和油脂。如果农药品种很多,GPC需要的,不多GPC可以用其他方法替代。
我在故我思
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Pesticide residue analyses in plant material by chromatographic methods: clean-up procedures and selective detectors
这篇文献在: http://www.instrument.com.cn/bbs/shtml/20080430/1243390/  一楼已经有版友热心的提供了,在此表示感谢!
这篇文献中提到了植物样品的净化及分离技术,有很多的参考文献,楼主需要的话可以看看。

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