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1.
A new method to determine pesticide residues in nuts is presented, in which the pesticides are extracted from samples with a small amount of ethyl acetate and anhydrous sodium sulfate. No additional cleanup or concentration steps are necessary. The extract is directly injected into the high-pressure liquid chromatograph, where preseparation of the pesticide residues from other components coextracted from the nuts is carried out using methanol/water as the eluent. The selected liquid chromatography fraction containing the pesticides is automatically transferred to the gas chromatograph using the through-oven transfer adsorption/desorption interface. The calculated limits of detection for each pesticide varied from 0.1 to 61.3 microg/kg. The repeatabilities of the analysis and the overall procedure (extraction and analysis) were satisfactory. No variations in the retention time were observed. The method was applied to the analysis of pistachio nut, peanut, walnut, hazelnut, and sunflower seed.  相似文献   

2.
A multiresidue solid phase extraction (SPE) method for the isolation and subsequent gas chromatographic determination of nonpolar organochlorine and polar organophosphorus pesticide residues in eggs is described. The method uses an acetonitrile extraction followed by an SPE cleanup using graphitized carbon black and aminopropyl SPE columns. Organophosphorus pesticides are determined by gas chromatography with flame photometric detection. After further cleanup of the extract using Florisil SPE columns, organochlorine pesticides are determined by gas chromatography with electron capture detection. Studies were performed using eggs containing both fortified and incurred pesticide residues. The average recoveries were 86-108% for 8 fortified organochlorine pesticide residues and 61-149% for 28 fortified organophosphorus pesticide residues.  相似文献   

3.
The applicability of supercritical fluid extraction (SFE) in pesticide multiresidue analysis (organohalogen, organonitrogen, organophosphorus, and pyrethroid) in soil samples was investigated. Fortification experiments were conducted to test the conventional extraction (solid-liquid) and to optimize the extraction procedure in SFE by varying the CO2 modifier, temperature, extraction time, and pressure. The best efficiency was achieved at 400 bar using methanol as modifier at 60 degrees C. For the SFE method, C-18 cartridges were used for the cleanup. The analytical screening was performed by gas chromatography equipped with electron-capture detection (ECD). Recoveries for the majority of pesticides from spiked samples of soil at different residence times were 1, 20, and 40 days at the fortification level of 0.04-0.10 mg/kg ranging from 70 to 97% for both methods. The detection limits found were <0.01 mg/kg for ECD, and the confirmation of pesticide identity was performed by gas chromatography-mass spectrometry in a selected-ion monitoring mode. Multiresidue methods were applied in real soil samples, and the results of the methods developed were compared.  相似文献   

4.
A novel and simple method for the determination of some pesticide residues in strawberries using both focused microwave-assisted extraction (FMAE) and solid-phase micro extraction (SPME), coupled with high-performance liquid chromatography (HPLC), has been developed. The pesticides were first extracted from strawberries with water and the assistance of focused microwaves at 30 W for 7 min. Then, an aliquot of the resulting aqueous extract was subjected to SPME with a 60-microm thick poly(dimethylsiloxane)/divinylbenzene (PDMS/DVB) fiber for 45 min at room temperature, with the solution being stirred at 1000 rpm. The extracted pesticides on the SPME fiber were desorbed into the SPME/HPLC interface for quantitative analysis with a diode array detector (DAD). The whole sample pretreatment procedure before chromatographic analysis did not use any organic solvents or involve any blending or centrifugation steps. The five compounds (carbendazim, diethofencarb, azoxystrobine, napropamide, and bupirimate) were chosen because they cannot be analyzed easily by GC. The efficiency of this relatively fast procedure was comparable to that of previously reported methods, with detection limits at low microg/kg levels and linear responses in the range from 0.05 to 1 mg/kg of pesticide in strawberries, with RSDs between 3 and 7.3%, depending on the analyte. In all but one case results obtained by this method for field-incurred samples were comparable to those obtained with traditional methods.  相似文献   

5.
Characterization of pesticide bioavailability, particularly in aged soils, is of continued interest because this information is necessary for environmental risk assessment. However, pesticide bioavailability in aged soils has been characterized by a variety of methods with limited success, due in part to methodological limitations. The objective of this study was to use solvent extraction methods to correlate simazine residue bioavailability in aged soils to simazine mineralization using a simazine-mineralizing bacterium. Soils from Brazil, Hawaii, and the midwestern United States were treated with UL-ring-labeled [14C]simazine and incubated for up to 8 weeks. At the end of each incubation period, soils were either incubated further, extracted with 0.01 M CaCl2, or extracted with aqueous methanol (80:20 v/v methanol/water). In a parallel experiment, after each incubation period, soils were inoculated with the bacterium Pseudomonas sp. strain ADP, which is capable of rapidly mineralizing simazine, and 14CO2 was determined. The inoculated soil samples were then extracted with 0.01 N CaCl2 and with aqueous methanol. This allowed for the evaluation of the bioavailability of aged simazine residues, without the contribution of simazine desorption from soil. Results of these studies indicated that simazine sorption to soil increased with aging and that amounts of simazine in aged soils extracted by 0.01 M CaCl2 and aqueous methanol were highly correlated to amounts of simazine mineralized by Pseudomonas sp. strain ADP. Consequently, 0.01 M CaCl2/methanol-extractable simazine in aged soils can be used to estimate bioavailable residues. This technique may be useful in determining the bioavailability of other s-triazine compounds in soils.  相似文献   

6.
Reduction of pesticide residues on produce by rinsing   总被引：6，自引：0，他引：6  
In 1997 this laboratory initiated a research program with the objective of examining the effect that rinsing of produce with tap water would have on pesticide residues. Samples were obtained from local markets and/or grown at our experimental farm. Because approximately 35% of produce from retail sources contains pesticide residues, growing and treating produce at an experimental farm had the advantage that all such samples contain pesticide residues. Pesticides were applied under normal field conditions to a variety of food crops and the vegetation was allowed to undergo natural weathering prior to harvest. The resulting samples contained field-incurred or "field-fortified" residues. This experimental design was employed to mimic as closely as possible real world samples. Crops were treated, harvested, and divided into equal subsamples. One subsample was processed unwashed, whereas the other was rinsed under tap water. The extraction and analysis method used was a multi-residue method developed in our laboratory. Twelve pesticides were included in this study: the fungicides captan, chlorothalonil, iprodione, and vinclozolin; and the insecticides endosulfan, permethrin, methoxychlor, malathion, diazinon, chlorpyrifos, bifenthrin, and DDE (a soil metabolite of DDT). Statistical analysis of the data using the Wilcoxon signed-rank test showed that rinsing removed residues for nine of the twelve pesticides studied. Residues of vinclozolin, bifenthrin, and chlorpyrifos were not reduced. The rinsability of a pesticide is not correlated with its water solubility.  相似文献   

7.
A new multiresidue method has been developed and validated for the simultaneous determination of 100 pesticide residues in olive oil. The determination of pesticide residues was carried out in only 19 min by gas chromatography coupled to tandem mass spectrometry using a triple quadrupole mass analyzer. The mass spectrometer was operated in electron ionization and the selection reaction monitoring mode was used, acquiring two or three fragmentation reactions per compound. Two extraction processes were studied, and an evaluation of the stability and sensitivity of the chromatographic system has been performed for the tested extraction procedures. The final proposed methodology was based on a liquid-liquid partition with an n-hexane/acetonitrile mixture followed by a gel permeation chromatography cleanup step. An adequate lineal relation was obtained in the studied concentration range (10-200 microg kg (-1)); the recovery values were in the range 70-110% for the two levels of concentration studied: 12 and 50 microg kg (-1). Precision values, expressed as relative standard deviation, were lower than 18% at the aforementioned spiking levels; detection limits, confirmation limits, and quantitation limits were below or equal to 1.9, 2.6, and 3.6 microg kg (-1), respectively. The developed methodology was applied to the analysis of pesticide residues in real samples of olive oil from the south of Spain.  相似文献   

8.
食品中的农药残留检测长期以来一直是一项艰巨的挑战,其杂质干扰多,残留含量低,传统的提取方法常常因为无法将杂质分离而影响检测结果。由于食品中杂质种类众多,农药的种类繁多且理化性质各异,新型农药日益涌现,所以对样品的前处理提出了更高的要求。近年来,QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)作为一种新型的提取方法,由于具有快速、简单、廉价、有效、可靠、安全的特点,成为国内外广泛采用的样品前处理新技术,在多种农药、医药、兽药的气相或液相色谱分析中已经得到广泛应用。本文就国内外对QuEChERS法在各类食品以及其他动植物性农产品的农药残留检测中的应用和方法的改进进行了综述,并对QuEChERS法在今后农药残留检测的应用前景以及发展方向进行了展望。  相似文献   

9.
A method for analysis of 37 pesticide residues in tea samples was developed and validated and was based on reversed-dispersive solid-phase extraction (r-DSPE) cleanup in acetonitrile solution, followed by liquid chromatography-electrospray tandem mass spectrometry determination. Green tea, oolong tea, and puer tea were selected as matrixes and represent the majority of tea types. Acetonitrile was used as the extraction solvent, with sodium chloride and magnesium sulfate enhancing partitioning of analytes into the organic phase. The extract was then cleaned up by r-DSPE using a mixture of multiwalled carbon nanotubes, primary secondary amine, and graphitized carbon black as sorbents to absorb interferences. Further optimization of sample preparation and determination allowed recoveries of between 70% and 111% for all 37 pesticides with relative standard deviations lower than 14% at two concentration levels of 10 and 100 μg kg(-1). Limits of quantification ranged from 5 to 20 μg kg(-1) for all pesticides. The developed method was successfully applied to the determination of pesticide residues in market tea samples.  相似文献   

10.
A liquid chromatographic method has been developed for simultaneous determination of residues of 10 sulfonamide drugs at 10 ppb and above in raw bovine milk. The method is based on a chloroform-acetone extraction, evaporation of organic phase, dissolution of residues in an aqueous potassium phosphate solution, and extraction of fatty residue into hexane. The aqueous layer is collected, filtered, injected onto an LC system, and detected by ultraviolet absorption at 265 nm. To elute all 10 sulfonamides isocratically, 2 chromatographic conditions are required. Seven sulfonamides can be quantitated with 12% methanol in the mobile phase; 4 sulfonamides can be quantitated with 30% methanol. Sulfamethazine, the most widely used sulfonamide, is detected on both systems. Recoveries are 44-87% for individual sulfonamides, with only 2 below 60%. Coefficients of variation are 3-13% at 10 ppb.  相似文献   

11.
采用MECC在线堆积同步检测茶叶中七种残留农药   总被引：4，自引：0，他引：4  
为解决茶叶中的痕量农药残留的快速检测问题,建立了一种基于胶束毛细管电泳在线堆积技术的茶叶中7种拟除虫菊酯类农药痕量残留的一次进样同步检测方法.通过参数优化,得到最优的柱上在线堆积浓缩操作工艺:以15%异丙醇、20%乙腈、60 mmol/L十二烷基硫酸钠(SDS)和50 mmol/L tris的混合物为背景缓冲溶液(BGS).茶叶的浸提液经过固相萃取净化吹干后,用1 mmol.L SDS溶解溶液残渣.进样100 s后施加反向电压,进行农药反向在线堆积,当电流恢复至正常分离时的95%时改变电压方向,进行正常分离.经过在线堆积浓缩,7种拟除虫菊酯类农药痕量残留堆积因子均高于17,回收率在82%以上,检测下限分别达到:功夫菊酯0.05 mg/kg、联苯菊酯0.05 mg/kg、百树菊酯0.05 mg/kg、高效氯氰菊酯0.05 mg/kg、溴氰菊酯0.2 mg/kg、二氯菊酯0.05 mg/kg、氰戊菊酯0.05 mg/kg,满足了2006年欧盟茶叶中拟除虫菊酯类农药残留的最低标准.  相似文献   

12.
A multiresidue method using liquid chromatography-time-of-flight mass spectrometry (LC-TOFMS) has been developed for the quantitative analysis of five widely used postharvest fungicides (carbendazim, thiabendazole, imazalil, prochloraz, and iprodione) and two of their transformation products (imazalil and prochloraz metabolites) in fruit juices. LC-TOFMS in positive electrospray ionization mode was used to quantify and confirm trace levels of these fungicides in fruit juices. The proposed method consists of a sample treatment step based on solid-phase extraction using hydrophilic-lipophilic-balanced polymer-based reverse-phase SPE cartridges (Oasis HLB) and methanol as an eluting solvent. Fruit-juice extracts spiked at different fortification levels (10 and 20 microg L(-1)) yielded average recoveries in the range of 71-109% with RSD (%) below 15%. Subsequent identification, confirmation, and quantitation were carried out by LC-TOFMS analysis. The confirmation of the target species was based on accurate mass measurements of protonated molecules ([M+H]+) and fragment ions, obtaining routine accuracy errors lower than 2 ppm in most cases. The obtained limits of detection (LODs) of the proposed method were in the range of 0.08-0.45 microg L(-1). Finally, the proposed method was successfully applied to the analysis of 23 fruit juice samples collected from different European countries and the United States, showing the potential applicability of the method in routine analysis. Over 50% of the samples tested contained pesticide residues, but relatively low concentration levels were found.  相似文献   

13.
A method was developed to determine pesticides in wines. The pesticides were extracted from the wine using solid-phase extraction on a polymeric cartridge, and the coextractives were removed with an aminopropyl-MgSO(4) cartridge. Analysis was performed using capillary gas chromatography with electron impact mass spectrometric detection in selective ion monitoring mode (GC-MSD/SIM). Three injections are required to analyze all 153 organohalogen, organonitrogen, organophosphate, and organosulfur pesticides and residues. Pesticides were confirmed by retention times of the target ions and three qualifier-to-target ion ratios. Detection limits for most of the pesticides were less than 0.005 mg/L, and quantitation was determined from approximately 0.01 to 5 mg/L. Spike recoveries were performed by fortifying red and white wines at 0.01 and 0.10 mg/L. At the 0.01 ppm level, the spike recoveries were greater than 70% for 116 and 124 pesticides (out of 153) in red and white wines, respectively, whereas at the higher spike concentration of 0.10 mg/L, the recoveries were greater than 70% for 123 and 128 pesticides in red and white wines, respectively. The recoveries of less than 70% were most likely from pesticide polarity or lability, resulting in the inefficient adsorption of the pesticide to the polymeric sorbent, ineffective elution of the pesticide from the sorbent, or thermal degradation of the pesticide under GC-MSD conditions.  相似文献   

14.
Characterization of pesticide bioavailability, particularly in aged soils, is of continued interest because this information is necessary for environmental risk assessment. The objective of this study was to correlate atrazine residue bioavailability in aged soils, as determined by solvent extraction methods, to atrazine mineralization by an atrazine-degrading bacterium. Webster clay loam and Zimmerman fine sand soils were treated with UL-ring-labeled [14C]atrazine and incubated for up to 8 weeks. At the end of each incubation period, soils were either not extracted, extracted with 0.01 M CaCl2, or extracted with 0.01 M CaCl2/aqueous methanol. Soils were then inoculated with the bacterium Pseudomonas sp. strain ADP, which is capable of rapidly mineralizing the atrazine ring. This allowed for the evaluation of the bioavailability of aged atrazine residues without the contribution of atrazine desorption from soil. Results of these studies indicated that the amounts of atrazine residues in aged soils extracted by 0.01 M CaCl2 and aqueous methanol were correlated to amounts of atrazine mineralized by Pseudomonas sp. strain ADP. Consequently, 0.01 M CaCl2/methanol extractable atrazine in aged soils may be used to estimate bioavailable residues, and this technique may be useful to determine the bioavailability of other compounds in soils, especially other triazine herbicides.  相似文献   

15.
A method based on disposable pipet extraction (DPX) sample cleanup and gas chromatography with mass spectrometric detection by selected ion monitoring (GC/MS-SIM) was established for 58 targeted pesticide residues in soybean, mung bean, adzuki bean and black bean. Samples were extracted with acetonitrile and concentrated (nitrogen gas flow) prior to being aspirated into DPX tubes. Cleanup procedure was achieved in a simple DPX-Qg tube. Matrix-matched calibrations were analyzed, and the limits of quantification (LOQ) of this method ranged from 0.01 mg kg(-1) to 0.1 mg kg(-1) for all target compounds. Coefficients of determination of the linear ranges were between 0.9919 and 0.9998. Recoveries of fortified level 0.02 mg kg(-1) on soybean, mung bean, adzuki bean and black bean were 70.2-109.6%, 69.1-119.0%, 69.1-119.8%, and 69.0-120.8%, respectively, for all studied pesticides. Moreover, pesticide risk assessment for all the detected residues in 178 market samples at Beijing market area was conducted. A maximum 0.958% of ADI (acceptable daily intake) for NESDI (national estimated daily intake) and 55.1% of ARfD (acute reference dose) for NESTI (national estimated short-term intake) indicated low diet risk of these products.  相似文献   

16.
Ethephon (2-chloroethylphosphonic acid) and fenoprop (2-(2,4,5-trichlorophenoxy) propionic acid) may be determined in the same apple sample. After extraction with methanol, 2 separate methylation procedures were required to quantitatively convert each compound. Ethephon was esterified with diazomethane and analyzed by a flame photometric detector in the P-mode. Fenoprop was esterified with boron trifluoride/methanol and analyzed by electron capture gas chromatography. Average recoveries were about 95% at 0.05 ppm for both compounds. The limit of detection was 0.05 ppm for ethephon and 0.01 ppm for fenoprop in a 1 g sample. The persistence of both compounds before and after harvest was studied. Ethephon and fenoprop were applied simultaneously to apple trees at the recommended concentrations of 300 and 20 ppm, respectively. Ethephon residues averaged 1.6, 0.75, and 0.4 ppm at 2 hr, 10 days, and after washing at 13 days, respectively. The corresponding fenoprop residues were 0.70, 0.025, and 0.024 ppm.  相似文献   

17.
An analytical procedure using accelerated solvent extraction and capillary gas chromatography with electron capture and flame photometric detections was developed to simultaneously determine residues of different pesticides in fruits and vegetables. Single laboratory validation of the method was carried out for 28 compounds selected from eight pesticide classes, in blank and fortified samples of fresh pear, cantaloupe, white potato, and cabbage. The method had to meet specific established validation criteria for regulatory purposes applicable to our laboratory. At each of the two fortification levels studied, 24 of the 28 pesticides gave recoveries of more than 70% with a coefficient of variation of less than 10%. With respect to existing procedures, the method showed acceptable limits of detection (from 0.0019 to 0.14 microg/g depending on the pesticide and matrix) while minimizing environmental concerns, time, and labor.  相似文献   

18.
A simple and efficient method is presented for the extraction, cleanup, and liquid chromatographic (LC) determination of oxamyl residues in potato tubers. Samples are extracted with methanol, partitioned into dichloromethane, and cleaned up using Sep-Pak Florisil cartridges. LC determination is performed using a Zorbax PSM 60 size exclusion column with an acetonitrile-water (1 + 9) mobile phase and UV detection at 254 nm. Recovery of oxamyl from spiked control tubers averaged 94.1 and 85.9% at fortification levels of 0.4 and 0.08 micrograms oxamyl/g tuber, respectively. The minimum detectable concentration of oxamyl by this method is 0.01 micrograms/g.  相似文献   

19.
Methods devised for oil extraction from avocado (Persea americana Mill.) mesocarp (e.g., Soxhlet) are usually lengthy and require operation at high temperature. Moreover, methods for extracting sugars from avocado tissue (e.g., 80% ethanol, v/v) do not allow for lipids to be easily measured from the same sample. This study describes a new simple method that enabled sequential extraction and subsequent quantification of both fatty acids and sugars from the same avocado mesocarp tissue sample. Freeze-dried mesocarp samples of avocado cv. Hass fruit of different ripening stages were extracted by homogenization with hexane and the oil extracts quantified for fatty acid composition by GC. The resulting filter residues were readily usable for sugar extraction with methanol (62.5%, v/v). For comparison, oil was also extracted using the standard Soxhlet technique and the resulting thimble residue extracted for sugars as before. An additional experiment was carried out whereby filter residues were also extracted using ethanol. Average oil yield using the Soxhlet technique was significantly (P < 0.05) higher than that obtained by homogenization with hexane, although the difference remained very slight, and fatty acid profiles of the oil extracts following both methods were very similar. Oil recovery improved with increasing ripeness of the fruit with minor differences observed in the fatty acid composition during postharvest ripening. After lipid removal, methanolic extraction was superior in recovering sucrose and perseitol as compared to 80% ethanol (v/v), whereas mannoheptulose recovery was not affected by solvent used. The method presented has the benefits of shorter extraction time, lower extraction temperature, and reduced amount of solvent and can be used for sequential extraction of fatty acids and sugars from the same sample.  相似文献   

20.
Fipronil is a pesticide suspected of having harmful effects on honey bees at microgram per kilogram levels. Considering the lack of methodology, it thus appeared to be necessary to develop a method for the determination of the lowest amounts of fipronil and its metabolites in pollen. This paper describes a new analytical method with a limit of quantification (LOQ) of 0.1 microg/kg for a representative sample weight of 5 g. In the case of a field study, this tool was used for checking the possible existence of fipronil and/or metabolites in pollen samples, but none of them contained residues higher than the LOQ. This three-step rapid method uses liquid-solid solvent extraction with mechanical grinding, followed by liquid-liquid partitioning and Florisil solid-phase extraction for the two cleanup steps. The quantification is made by liquid chromatography with electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS). Indeed, combined with an adequate sample treatment, this technique offers good sensitivity and selectivity in such a complex matrix. The method has given good recoveries of 74-104% with relative standard deviations of 5.6-18.2%.  相似文献   

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