Contributions to the ethyl acetate application in residue analysis

Summary Atrazine was extracted from two weathered soil samples with the proposed micro extraction method using ethyl acetate as the extracting agent. The results were compared with other extraction methods tested. The proposed micro method was equally effective as the micro on-line method using acetone for the extraction and more effective than the Soxhlet extraction using acetone and methanol. Therefore, the proposed micro ethyl acetate method can be used for routine analysis.     

分散固相萃取/高效液相色谱-串联质谱法检测大葱中虫酰肼、涕灭威及其衍生物的农药残留

采用分散固相萃取法净化(DSPE),高效液相色谱-串联质谱法(HPLC-MS/MS)在分时段多反应监测模式下对大葱中的虫酰肼、涕灭威及其衍生物进行测定,外标法定量,并对比了乙酸乙酯和乙腈作为提取剂的提取效果.结果表明,采用乙腈为提取剂时,4种农药在10～120μg/L范围内线性关系良好,且方法的定量下限(LOQ)均低于...     

Determination of inorganic anions in ethyl acetate by in-line hollow fiber membrane extraction with ion chromatography

In this work,a novel hollow fiber membrane extractor was set up to extract inorganic anions from ethyl acetate using deionized water.Inorganic anions in slightly soluble organic solvents can be determined by the in-line hollow fiber membrane extractor coupled with ion chromatography at first time.Different aspects of the extraction procedure such as magnetic stirring speed, extraction flow rate and extraction time were optimized to achieve high extraction efficiency and good separation results. Satisfact...     

Comparison of methods for extraction of ethyl carbamate from alcoholic beverages in gas chromatography/mass spectrometry analysis

A procedure to analyze ethyl carbamate (EC) by gas chromatography/mass spectrometry was optimized and validated. Deuterated EC (d5-EC) was added to the samples as an internal standard followed by extraction with polystyrene crosslinked polystyrene cartridges using minimal volumes of ethyl acetate. The EC response was measured in selective ion monitoring (SIM) mode and found to be linear in the range between the limit of quantitation (10 micro/L) and 1000 microg/L. EC recoveries varied from 92 to 112%, with the average value of 100 +/- 8%. The procedure compared well (r2 = 0.9970) with the existing AOAC Official Method with the added benefits of minimal solvent usage and reduced matrix interferences.     

Quantitation of SR 27417 in human plasma using electrospray liquid chromatography-tandem mass spectrometry: A study of ion suppression

The effect of coeluting matrix compounds on the quantitation of SR 27417 in human plasma using electrospray liquid chromatography-tandem mass spectrometry has been examined. During the method development stage of this assay, plasma samples spiked with the analyte at 100 pg/mL were extracted using three different procedures: a hexane liquid-liquid extraction, an ethyl acetate back-extraction, and a solid phase extraction. Ion intensity of the analyte was found to be related inversely to the percent ionization of coeluting matrix components as evidenced by full scan spectra. The ethyl acetate back-extraction, which contained the fewest coeluting components, resulted in the highest ion intensity for the analyte. An assay comparison was done by using the liquid-liquid hexane and the ethyl acetate back-extractions for sample preparation. Replicate 1-mL samples (n=5) at 11 concentrations from 5 to 2000 pg/mL were extracted and analyzed. The results for the ethyl acetate back-extracted samples were acceptable from 2000 to 5 pg/mL with accuracy ranging from ?11.6 to 2.61% of the nominal concentrations. In contrast, the hexane liquid-liquid method had poor accuracy and precision below 20 pg/mL. The difference is explained by suppression of analyte ion intensity. These results are consistent with the current theory of electrospray ionization.     

Determination of antibiotics such as macrolides,ionophores and tiamulin in liquid manure by HPLC–MS/MS

A method for the analysis of several macrolide and ionophore antibiotics as well as tiamulin in liquid manure was developed. Reversed-phase liquid chromatography and atmospheric pressure chemical ionisation (APCI) tandem mass spectrometry was used for detection.High-performance liquid chromatographic (HPLC) separation of the antibiotics was achieved in 35 min. The analytes were extracted with ethyl acetate and the extracts were cleaned up by solid-phase extraction on a diol SPE cartridge. Recovery experiments with spiked liquid manure concentrations varying from 6 to 2,000 microg kg(-1) gave constant recovery rates. The recovery rates for the macrolides erythromycin, roxithromycin and oleandomycin were 75-94%, that for the ionophore salinomycin was 119%, while that for the pleuromutilin tiamulin was 123%, when using a macrolide internal standard. The relative standard deviation was found to be 15-36% and the limits of detection were 0.4-11.0 micro g kg(-1).The maximum concentrations found in manure samples were 43 micro g kg(-1) for tiamulin and 11 micro g kg(-1) for salinomycin.     

Multiresidue analysis of pesticides in vegetables and fruits using a high capacity absorbent polymer for water

A single extraction and a single clean-up procedure was developed for multi-residue analysis of pesticides in non-fatty vegetables and fruits. The method involves the use of a high capacity absorbent polymer for water as a drying agent in extraction from wet food samples and of a graphitized carbon column for clean-up. A homogeneously chopped food sample (20 g) and polymer (3 g) were mixed to absorb water from the sample and then 10 min later the mixture was vigorously extracted with ethyl acetate (100 ml). The extract (50 ml), separated by filtration, was loaded on a graphitized carbon column without concentration. Additional ethyl acetate (50 ml) was also eluted and both eluates were concentrated to 5 ml for analysis. The procedure for sample preparation was completed within 2 h. In a recovery test, 107 pesticides were spiked and average recoveries were more than 80% from asparagus, orange, potato and strawberry. Most pesticides were recovered in the range 70-120% with usually less than a 10% RSD for six experiments. The results indicated that a single extraction with ethyl acetate in the presence of polymer can be applied to the monitoring of pesticide residues in foods.     

Alkannin/shikonin mixture from roots of Onosma echioides (L.) L.: extraction method study and quantification

This work reports the extraction procedures of alkannin/shikonin mixture from roots of six populations of Onosma echioides, by means of three extraction techniques: Soxhlet extraction, maceration and rapid solid-liquid dynamic extraction (RSLDE). Five solvents with different polarity (hexane, petroleum ether, chloroform, ethyl acetate, methanol) were also studied. Analysis of the extracts was performed by an HPLC-DAD (diode array detector) system. The most efficient extraction technique was Soxhlet procedure using ethyl acetate for 6 h. Studied samples of O. echioides showed an alkannin/shikonin content in the range of 0.02-0.24 mg/kg. Other naphthoquinone derivatives (deoxyalkannin/deoxyshikonin and 5,8-dihydroxy-2-(4-methyl-6-oxo-5,6-dihydro-2H-pyran-2-yl)-[1,4]naphthoquinone and arnebin-6) were found for the first time in O. echioides and characterized in the extracts using HPLC-MS apparatus equipped with an ESI ionization source.     

Validation and uncertainty analysis of a multi-residue method for pesticides in grapes using ethyl acetate extraction and liquid chromatography-tandem mass spectrometry

A method was validated for the multi-residue analysis of 82 pesticides in grapes at 相似文献   

The extraction of iridium and platinum from organic solvents by polyurethane foam

The feasibility of extracting iridium and platinum from organic solvents onto polyurethane foam was studied. Distribution ratios obtained were 1.1 x 10(4) for the extraction of iridium from ethyl acetate, 225 for the extraction of iridium from acetone and 4.8 x 1O(3) for the extraction of platinum from ethyl acetate. Capacities of about 16% w/w were obtained for extraction of iridium from ethyl acetate, and about 2.4% for extraction from acetone.     

Comparison of an acetonitrile extraction/partitioning and "dispersive solid-phase extraction" method with classical multi-residue methods for the extraction of herbicide residues in barley samples

An acetonitrile/partitioning extraction and "dispersive solid-phase extraction (SPE)" method that provides high quality results with a minimum number of steps and a low solvent and glassware consumption was published in 2003. This method, suitable for the analysis of multiple classes of pesticide residues in foods, has been given an acronymic name, QuEChERS, that reflects its major advantages (quick, easy, cheap, effective, rugged, safe). In this work, QuEChERS method, which was originally created for vegetable samples with a high amount of water, was modified to optimise the extraction of a wide range of herbicides in barley. Then, it was compared with known conventional multi-residue extraction procedures such as the Luke method, which was simplified and shortened by eliminating the Florisil clean-up (mini Luke) and the ethyl acetate extraction, which involves a subsequent clean-up by gel permeation chromatography (GPC) and which is the official extraction method used by some of European authorities. Finally, a simple acetone extraction was carried out to check the differences with the other three methods. Extracts were analysed by gas chromatography-time-of-flight mass spectrometry (GC-TOF/MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Mini Luke was significantly more effective for the extraction of non-polar and medium-polar compounds, but the best recoveries for polar compounds were achieved by QuEChERS and ethyl acetate methods. QuEChERS was the only method that provided an overall recovery value of 60-70% for non-, medium- and polar compounds, with some exceptions due to co-eluted matrix interferences. Clean-up by dispersive SPE was effective and did not differ so much with ethyl acetate extracts considering that QuEChERS clean-up step is much easier and less time-consuming. As a conclusion, it resulted to be the most universal extraction method by providing a well-defined phase separation without dilution and achieving acceptable recoveries in average including the extraction of the always difficult acidic herbicides. However, recoveries were not as good as required for validation purposes suggesting that residues are prone to strong matrix interactions in dry samples as barley and further method adaptation incrementing solvent strength, extraction time or more acidic or basic conditions is needed in order to achieve a complete extraction.     

Substoichiometric determination of zinc with potassium ethyl xanthate

A rapid radiochemical method has been designed for the determination of microgram quantities of zinc, based on the substoichiometric isotope dilution, using potassium ethyl xanthate as the extraction reagent. pH 5.5 in acetate buffers and chloroform as the extractant were found to be suitable for quantitative substoichiometric extraction. The influence of the diverse ions on the extraction was studied. The zinc contents of a medicinal preparation and biological samples were determined by the present method.     

Determination of melatonin and its precursors and metabolites using capillary electrophoresis with UV and fluorometric detection

A micellar electrokinetic chromatography method has been developed for simultaneous determination of melatonin and its precursors and metabolites. A 20 mM borate buffer pH 9.5 with 50 mM SDS served as the electrolyte. Tryptophan, 5-methoxyindoleacetic acid, 6-hydroxymelatonin, melatonin, serotonin, and 5-methoxytryptamine were baseline separated in less than 13 min. The limits of detection for UV detection and fluorometric detection based on native fluorescence of analytes were at the sub-ppm level. The proposed method with UV detection was applied to melatonin content control in pharmaceutical tablets with a precision expressed as RSD (n = 7) = 1.6%. For biological samples extraction with chloroform and ethyl acetate was examined. With ethyl acetate and chloroform recoveries of 87.2% and 82.1% melatonin, respectively, were obtained from plasma samples. The recovery of melatonin from spiked urine samples was 80.0% for ethyl acetate and 82.5% for chloroform. Fluorometric detection provides about two-fold improvement over UV in the detection of melatonin and minor improvements for three other analytes, but is much poorer than UV for tryptophan and 6-hydroxymelatonin in applied conditions.     

Analysis of 28 insecticides in curry leaves (Murraya koenigii L.) by gas chromatography and gas chromatography–mass spectrometry

A simple and efficient method was developed for analysis of 28 insecticides (organochlorines, organophosphates and synthetic pyrethroids) in curry leaves (Murraya koenigii L.). The extraction of the analytes was carried out with acidified acetonitrile and purification with magnesium sulphate, primary secondary amine along with graphitised carbon black to remove excess chlorophyll content in curry leaves. Acetonitrile extracts were changed into hexane + acetone (9 + 1) and hexane + toluene (9 + 1) in the final step. In another method ethyl acetate was used for extraction and purification was carried out as above. The analytes in the samples were determined by gas chromatography (GC) and confirmed by gas chromatography–mass spectrometry (GC–MS). Use of ethyl acetate increased the recovery of the analytes, but co-extractive interference led to higher GC maintenance. Acidified acetonitrile was found to be a better extraction solvent compared with ethyl acetate. The use of hexane:toluene (9:1) as exchange solvent increased the recovery of organochlorine insecticides compared with hexane:acetone (9:1). The limit of quantification (LOQ) of the method was 0.01 mg kg^?1 for organochlorine insecticides and 0.05 mg kg^?1 for organophosphates and synthetic pyrethroids. The recoveries of organochlorines were within 70.36–82.45%; organophosphates, 82.54–90.93% and synthetic pyrethroids, 88.45–90.71% at the LOQ level. The method developed was found suitable for analysis of real samples of curry leaves. The pesticides detected in curry leaves collected from the retail market were mainly organophosphates and synthetic pyrethroids.     

Comparison of a GC Method and Two HPLC Methods for the Determination of p-Hydroxyphenytoin in Urine

Abstract

Three chromatographic methods for determining p-hydroxy-phenytoin (p-HPT) in urine were compared: (1) GC with derivatisation of the samples, (2) HPLC after extraction with ethyl acetate and (3) HPLC using a column switching system for direct injection of samples. In all three methods the p-HPT glucuronides were first hydrolysed using concentrated mineral acid at boiling point. For method (1) the acidic hydrolysate was adjusted to pH 7–8.5. Benzenetetrahydrofuran was used for extraction of p-HPT. The extract was evaporated to dryness, taken up in trimethyl-aniliniumhydroxide and injected. For method (2) the acidic hydrolysate was buffered with tri-sodium phosphate. An aliquot of the buffered solution was extracted with ethyl acetate. The extract was evaporated to dryness, taken up in methanol and injected. For method (3) the hydrolysate was diluted with water/acetonitrile (9:1), centrifuged and directly injected onto the pre-column for the sample washing step.     

Simultaneous determination of nitroimidazole residues in honey samples by high-performance liquid chromatography with ultraviolet detection

A rapid and sensitive high-performance liquid chromatography (LC) method was developed for the simultaneous determination of metronidazole (MNZ), dimetridazole (DMZ), ronidazole (RNZ), tinidazole (TNZ), and 2-hydroxymethyl-1-methyl-5-nitroimidazole (HMMNI) in honey. After extraction with ethyl acetate and evaporation, the residue containing the nitroimidazoles was dissolved in ethyl acetate-hexane and subjected to solid-phase extraction cleanup by amine extraction columns. The effluent was evaporated to dryness, and residues were dissolved and determined by LC with an ultraviolet detector set at 315 nm. The limits of detection were 1.0-2.0 ng/g for MNZ, DMZ, RNZ, TNZ, and HMMNI in honey. Average recoveries ranged from 71.5-101.4% in honey fortified at 10, 20, 50, and 100 ng/g. The method was validated for the analysis of real honey samples.     

蔬菜中有机氯农药残留的超临界流体提取和气相色谱法测定

建立了用超临界流体萃取、气相色谱测定韭菜中百菌清、艾氏剂、狄氏剂、异狄氏剂残留量的方法。样品与无水硫酸镁混合后进行萃取。用正交设计法选择萃取条件,最佳条件为压力３０．４ＭＰａ,温度４０℃。静态萃取时间１ｍｉｎ,ＣＯ２用量１５ｍＬ,收集液为乙酸乙酯。     

Determination of triazines and organophosphorus pesticides in water samples using solid-phase extraction.

Octadecyl (C18)-bonded porous silica was evaluated for the extraction of triazine and organophosphorus pesticides from natural water. The extraction results showed an effective performance when 11 of water was passed through small glass columns containing 500 mg of 50-100-microns C18 bonded porous silica. The adsorbed compounds were removed with ethyl acetate, evaporated to 200 microliters and determined by gas chromatography. The overall average recoveries were greater than 85% except for dimethoate and trichlorfon. Application of this procedure to the analysis of natural water samples gave results that agree well with those obtained by solvent extraction methods.     

固相萃取-气相色谱法测定水中毒死蜱

水样中的毒死蜱经全自动固相萃取仪萃取、乙酸乙酯洗脱后,用气相色谱火焰光度检测法测定,以保留时间定性,外标法定量．结果表明：选用ENVI-18小柱萃取、乙酸乙酯洗脱,在2mL／min的过水速率下取得了良好的回收率．方法的线性范围为0．25～4．0mg／L．r为0．9998,回收率为88．6％～100．6％,相对标准偏差为2．58％～7．34％,最低定量浓度为2．5μg／L．本方法快速、灵敏、准确,并能够很好的排除干扰,可以满足水中痕量毒死蜱的测定．     

Determination of inorganic anions in ethyl acetate by ion chromatography with an electromembrane extraction method

In this work, the determination of inorganic anions in slightly water-soluble organic solvents (ethyl acetate) was realized by ion chromatography (IC) with a novel-efficient electromembrane extraction method. From an 8 mL ethyl acetate sample, three inorganic anions migrated through the pores of a polypropylene hollow fiber membrane, and into deionized water inside the lumen of the hollow fiber by the application of 600 V. The transport was forced by an electrical potential difference sustained over the liquid membrane, resulting in electrokinetic migration of inorganic anions from the donor compartment to the acceptor solution. After the electromembrane extraction, the acceptor solution was analyzed by IC with a sodium carbonate-sodium bicarbonate eluent. The applied voltage, stirring speed, and extraction time for controlling the extraction efficiency were optimized. Within 10 min of operation at 600 V, chloride, bromide, and sulfate were extracted with recoveries in the range 76-110%, which corresponded to a linear range of 0.01-1 mg/L. The procedure was applied to the analysis of inorganic anions in a real ethyl acetate sample and expands onto other slightly water-soluble organic solvents.