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 DetectionV. 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 MatrixesAuthor(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/。