Cloud point extraction preconcentration prior to high-performance liquid chromatography coupled with cold vapor generation atomic fluorescence spectrometry for speciation analysis of mercury in fish samples

A cloud point extraction methodology was developed for simultaneous preconcentration of Hg(II), methylmercury (MeHg), ethylmercury (EtHg), and phenylmercury (PhHg) prior to reversed-phase high-performance liquid chromatography (HPLC) on-line coupled with cold vapor atomic fluorescence spectrometry for speciation analysis of mercury in fish. The four mercury species were taken into complexes with ammonium pyrrolidine dithiocarbamate (APDC) in aqueous nonionic surfactant Triton X-114 medium and concentrated in the surfactant-rich phase by bringing the solution to the temperature of 40 degrees C. Baseline separation of the enriched complexes was achieved on an RP-C(18) column with a mixture of methanol, acetonitrile, and water (65:15:20, v/v) containing 200 mmol L(-1) HAc (pH 3.5) as the mobile phase. An on-line postcolumn oxidation of the effluent from HPLC, in the presence of K2S2O8 in HCl, was applied in the system followed by an optimal cold vapor generation of mercury species. The variables affecting the complexation and extraction steps were examined. The preconcentration of 10 mL of solution with 0.08% w/v Triton X-114 and 0.04% w/v APDC at pH 3.5 gave enrichment factors of 29, 43, 80, and 98 for MeHg, EtHg, PhHg, and Hg(II), respectively. Low detection limits (S/N = 3) were obtained, ranging from 2 to 9 ng L(-1) (as Hg) for all species. The developed method was successfully applied to the speciation of mercury in real fish samples.     

Novel field sampling procedure for the determination of methiocarb residues in surface waters from rice fields.

Methiocarb was extracted from surface water samples collected at experimental rice field sites in Louisiana and Texas. The sampling system consisted of a single-stage 90-mm Empore extraction disk unit equipped with a battery-powered vacuum pump. After extraction, the C-18 extraction disks were stored in an inert atmosphere at -10 degrees C and shipped overnight to the laboratory. The disks were extracted with methanol and the extracts analyzed by reversed-phase high-performance liquid chromatography with a methanol/water mobile phase. Methiocarb was detected by ultraviolet absorption at 223 nm and quantified with the use of calibration standards. Recoveries from control surface water samples fortified at 5.0, 10, 50, and 100 ng/mL methiocarb averaged 92 +/- 7%. A method limit of detection for methiocarb in rice field surface water was estimated to be 0.23 ng/mL at 223 nm.     

Pressurized liquid extraction and HPLC quantification of folic Acid in fortified wheat flours

A pressurized liquid extraction (PLE) method using phosphate buffer as solvent was applied for folic acid (FA) extraction from fortified wheat flours and was compared to a standard solid-liquid extraction (SLE) method. Extracted FA was quantified by reverse phase high-performance liquid chromatography (RP-HPLC) hyphenated with a phenyl column and an absorption photometric detector (λ = 280 nm). Detection and quantification limits were 0.12 and 0.4 ng, respectively, corresponding to 0.06 and 0.2 μg g(-1) of analyzed wheat flour. Equivalent FA contents were found by both extraction methods, but a single PLE allowed a total recovery of FA content, whereas at least three successive SLEs were needed to achieve a total recovery of FA. The obtained results indicated that PLE is a rapid and efficient technique for FA extraction from fortified wheat flour.     

Effect of Tempering Conditions on Milling Performance and Flour Functionality

Tempering conditions of wheat grain change the quality of the flour, yet most experimental milling systems use a standard tempering without optimization. The effect of tempering condition on milling performance and flour functionality for soft red winter (SRW) wheat grain was tested by measuring flour yield, ash, polyphenol oxidase (PPO), and solvent retention capacity (SRC) in grain samples from three SRW cultivars (Roane, Cyrus, and Severn). Tempering was conducted with a full factorial design of initial wheat moisture, tempered wheat moisture, tempering temperature, and tempering time at two levels. Tempered wheat moisture had the largest effect on milling performance and flour functionality. Flour yield was more reduced for all samples tempered at 15% moisture than for samples tempered to 12% moisture. Flour quality of the 15% tempered sample was better than the 12% tempered samples due to less bran contamination as measured by flour ash and PPO. Increasing the tempering moisture increased flour sucrose SRC and lactic acid SRC but reduced sodium carbonate SRC for samples. Changing tempered wheat moisture changed flour yield and quality much more than did changing the length of time for tempering, the temperature at wheat is tempered, or differences in the initial moisture of the wheat before tempering. The last three effects could be used to improve flour yield in both the 12 and 15% tempered wheat treatment but the detrimental effects of these treatments on flour quality were minimal when combined with the 15% tempered wheat moisture treatment.     

Liquid chromatographic method for determination of citreoviridin in corn and rice

Citreoviridin, a neurotoxic mycotoxin, has been found as a natural contaminant in corn left unharvested in the southeastern United States and in rice of several Asian countries, including Japan. A reliable analytical method for the quantitative determination of citreoviridin in corn and rice is described. Corn or rice is extracted with dichloromethane, and the extract is partially purified on silica and amino solid-phase extraction (SPE) columns. The extract is analyzed for citreoviridin by normal-phase liquid chromatography, using a mobile phase of ethyl acetate-hexane (75 + 25) at 1.5 mL/min and a fluorescence detector to measure the yellow fluorescence (388 nm excitation, 480 nm emission). With a 100 microL injection loop, the relationship between concentration and injection volume is linear for 20-60 microL injections. Recoveries of citreoviridin added to yellow corn at 10-50 ng/g were 91.0-96.9%; recoveries from white corn (10-50 ng/g added) were 96.8-102.8%. Recoveries of 5000 ng/g added to white corn were 89.0%, indicating that heavily contaminated samples can be assayed by the method. Minimum detection limits were 10 ng for citreoviridin standard and 2 ng/g for citreoviridin added to corn. White rice fermented with Penicillium citreo-viride (1524 ppm) was mixed with and serially diluted with uncontaminated ground corn to obtain citreoviridin-contaminated corn (ca 25 ppb). When the samples were assayed by the method, a mean level of 24.4 +/- 1.65 ppb (6.5% coefficient of variation) was obtained. Four fermented rice food samples and 3 commercial rice samples were investigated.(ABSTRACT TRUNCATED AT 250 WORDS)     

Accelerated solvent extraction of alkylresorcinols in food products containing uncooked and cooked wheat

This research focuses on the overall extraction process of alkylresorcinols (ARs) from uncooked grains and baked products that have been processed with wheat, corn, rice, and white flour. Previously established extraction methods developed by Ross and colleagues, as well as a semiautomated method involving accelerated solvent extraction (ASE), were applied to extract ARs within freshly ground samples. For extraction of alkylresorcinols, nonpolar solvents such as ethyl acetate have been recommended for the extraction of uncooked foods, and polar solvents such as 1-propanol:water (3:1 v/v) have been recommended for the extraction of baked foods that contain rye, wheat, or other starch-rich grains. A comparison of AR extraction methods has been investigated with the application of gas chromatography and a flame ionization detector (GC-FID) to quantify the AR content. The goal of this research was to compare the rapid accelerated solvent extraction of the alkylresorcinols (ASE-AR) method to the previous manual AR extraction methods. Results for this study as well as the investigation of the overall efficiency of ASE-AR extraction with the use of a spiking study indicated that it can be comparable to current extraction methods but with less time required. Furthermore, the extraction time for ASE (approximately 40 min) is much more convenient and less tedious and time-consuming than previously established methods, which range from 5 h for processed foods to 24 h for raw grains.     

End-Use Quality of Flour from Rhyzopertha dominica Infested Wheat

The objective of this study was to evaluate how Rhyzopertha dominica infestation of stored wheat grain affects the rheological and baking properties of bread made with the milled flour. Wheat samples were infested with R. dominica and stored for up to 180 days at room temperature. Every 45 days, samples of wheat were collected and evaluated for insect population and flour yield. Flour milled from these wheat samples was evaluated for color reflectance, pH, fat acidity, and rheological properties which were measured by a farinograph. Loaves of bread were baked using a straight-dough procedure. Volume, height, and weight of the loaves were evaluated. None of the analyses performed on the control wheat flours showed any changes during the storage period, and they were similar to the initial wheat. The insect population increased during storage of the wheat up to 90 days, and the flour yield decreased with the storage up to 180 days. Flours from insect-infested wheat absorbed more water than did flours from control wheat. Dough stability and dough development times of infested flours decreased. Bread volume showed a progressive decline throughout the storage experiment. In conclusion, flour from insect-infested wheat exhibited changes in rheological properties such as dough stability, dough development times, water absorption, and mixing stability; bread had an offensive odor; and volume and loaf characteristics were negatively affected.     

Antioxidants and antioxidant activity of several pigmented rice brans

This study investigated the antioxidant content and activity of phenolic acids, anthocyanins, α-tocopherol and γ-oryzanol in pigmented rice (black and red rice) brans. After methanolic extraction, the DPPH free radical scavenging activity and antioxidant activity were measured. The pigmented rice bran extract had a greater reducing power than a normal rice bran extract from a long grain white rice. All bran extracts were highly effective in inhibiting linoleic acid peroxidation (60-85%). High-performance liquid chromatography (HPLC) analysis of antioxidants in rice bran found that γ-oryzanol (39-63%) and phenolic acids (33-43%) were the major antioxidants in all bran samples, and black rice bran also contained anthocyanins 18-26%. HPLC analysis of anthocyanins showed that pigmented bran was rich in cyanidin-3-glucoside (58-95%). Ferulic acid was the dominant phenolic acid in the rice bran samples. Black rice bran contained gallic, hydroxybenzoic, and protocatechuic acids in higher contents than red rice bran and normal rice bran. Furthermore, the addition of 5% black rice bran to wheat flour used for making bread produced a marked increase in the free radical scavenging and antioxidant activity compared to a control bread.     

Separation and purification of tricin from an antioxidant product derived from bamboo leaves

Tricin (5,7,4'-trihydroxy-3',5'-dimethoxyflavone) occurs in its glycosidic form in rice bran and other grass species such as wheat, barley, and maize. Tricin is considered sufficiently safe for clinical development as a cancer chemopreventive agent, therefore it can be used for cancer prevention. This study established a new method for the preparation of tricin from bamboo leaves as an alternative to traditional methods such as chemical synthesis via the Baker-Venkata-Raman reaction between acetylsyringic acid and phloroacetophenone. Tricin was prepared from an antioxidant product that was derived from bamboo leaves (AOB) by extraction with aqueous ethanol. A concentrated solution of this product was obtained and then processed by polystyrene (AB-8) resin column chromatography and preparative high-performance liquid chromatography (HPLC) with 30% (v/v) acetonitrile in 1% (v/v) acetic acid as the mobile phase. The collected tricin-rich fraction was further sequentially purified by dialysis membrane separation and drowning-out crystallization methods. The purity was assessed by analytical HPLC with 25% (v/v) acetonitrile in 1% (v/v) acetic acid as the mobile phase, and the chemical confirmation was evaluated by infrared, mass, nuclear magnetic resonance, and ultraviolet spectroscopies. Tricin (3.09 g) was prepared from 174 g of a crude column chromatography fraction obtained from 5 L of AOB concentrated solution. The present method is appropriate for preparing quantities of pure tricin, which can be used for the quantification of tricin in various plant herbs and further for pharmaceutical/biomedical applications and evaluation.     

Simultaneous determination of ochratoxin A and cyclopiazonic,mycophenolic, and tenuazonic acids in cornflakes by solid-phase microextraction coupled to high-performance liquid chromatography

A solid-phase microextraction (SPME) method, coupled to liquid chromatography with diode array UV detection (LC-UV/DAD), for the simultaneous determination of cyclopiazonic acid, mycophenolic acid, tenuazonic acid, and ochratoxin A is described. Chromatographic separation was achieved on a propylamino-bonded silica gel stationary phase using acetonitrile/methanol/ammonium acetate buffer mixture (78:2:20, v/v/v) as mobile phase. SPME adsorption and desorption conditions were optimized using a silica fiber coated with a 60 microm thick polydimethylsiloxane/divinylbenzene film. Estimated limits of detection and limits of quantitation ranged from 3 to 12 ng/mL and from 7 to 29 ng/mL, respectively. The method has been applied to cornflake samples. Samples were subjected to a preliminary short sonication in MeOH/2% KHCO(3) (70:30, v/v); the mixture was evaporated to near dryness and reconstituted in 1.5 mL of 5 mM phosphate buffer (pH 3) for SPME followed by LC-UV/DAD. The overall procedure had recoveries (evaluated on samples spiked at 200 ng/g level) ranging from 74 +/- 4 to 103 +/- 9%. Samples naturally contaminated with cyclopiazonic and tenuazonic acids were found; estimated concentrations were 72 +/- 9 and 25 +/- 6 ng/g, respectively.     

SDS-Protein Gel Test for Prediction of Bread Loaf Volume

Flour dispersed in aqueous solutions of sodium dodecyl sulfate (SDS) forms a proteinaceous gel when centrifuged at high speed. The conventional methodology for SDS gel testing was modified to develop a small-scale (<1 g of flour or wheat meal) screening test for evaluation of the protein quality of wheat for breadmaking. The principal modification involved centrifugation with a swinging-bucket rotor to facilitate direct measurement of gel height, which is the primary test parameter. The effects of suspension temperature and time, centrifugation speed, sample size, and sieving of ground wheat or flour on the efficacy of the test were examined. Gel height, wet weight, and protein content were assessed as test parameters. In the standard test procedure that was developed, 0.67 g of flour or ground whole wheat was dispersed in 13.5 mL of 1.5% SDS solution for 15 min at 20°C, followed by centrifugation at 80,000 × g for 30 min. The test was evaluated using seven Canadian commercial wheat flours with diverse breadmaking quality. For the samples, gel height was strongly related to loaf volume (R² = 0.89 and 0.95 for flour and ground wheat, respectively). Sieving flour through a 75-μm sieve slightly increased the predictive power of the test (R² = 0.94). SDS gel height gave better discrimination of samples for prediction of loaf volume than did the traditional SDS sedimentation test. The performance of the sedimentation test improved when sieved ground wheat was used. The relationship between gel height or protein content and flour protein content was comparatively poor (R² = 0.25). The SDS gel test appears to primarily measure the effects of flour protein quality.     

Effect of Different Wheat Classes and Their Flour Milling Streams on Textural Properties of Flour Tortillas

Wheat flour tortillas were made from flour streams of three wheat cultivars: Jagger hard red winter wheat, 4AT-9900 hard white winter wheat, and Ernie soft red winter wheat. Wheat samples were milled on a Miag experimental mill. Twelve flour streams and one straight-grade flour were obtained. Tortillas were made from each flour stream and the straightgrade flour by the hot-press method. Tortilla stretchability and foldability were evaluated by a texture analyzer and six panelists, respectively. Flour protein and water absorption affected tortilla texture. The foldability evaluated by panelists was positively correlated with flour protein content, farinograph water absorption, and damaged starch (P < 0.05). The 2BK and 3BK streams of hard wheat produced tortillas with strong stretchability and good foldability. Middling streams of hard wheat yielded tortillas with lighter color and less stretchability. Under the conditions tested in this study, soft wheat flours were not good for producing flour tortillas.     

Liquid chromatographic determination of pentaerythritol tetranitrate in pharmaceuticals: collaborative study

A liquid chromatographic (LC) method for the determination of pentaerythritol tetranitrate (PETN) in pharmaceutical formulations and the bulk drug triturate was evaluated in an interlaboratory study that included 12 participating laboratories. The procedure involves extraction of the active ingredient with mobile phase, followed by filtration of the extract and reverse-phase liquid chromatography using an octadecylsiliane bonded phase column and UV detection at 230 nm. The mobile phase composition is 35% water in acetonitrile (v/v). Three bulk drug samples (20, 20, and 35% PETN), 2 commercial tablet formulations (20 and 80 mg PETN/tablet), and 1 commercial capsule formulation (45 mg PETN/capsule) were analyzed in duplicate by the proposed method. Repeatability (sr, RSDr) and reproducibility (SR, RSDR) based on peak height measurement for these samples ranged from 0.0066 to 0.1806 (0.53-3.36%) and 0.0165 to 0.2075 (0.76-3.86%), respectively. Results for peak area measurements ranged from 0.0145 to 0.2011 (0.93-3.74%) and 0.0231 to 0.2091 (1.28-3.89%), respectively. The method has been approved interim official first action by AOAC.     

Gas chromatographic method for ethylene dibromide in grains and grain-based products: collaborative study

Nine laboratories analyzed samples of whole grain, intermediate, and ready-to-eat products for ethylene dibromide (EDB) residues. Supplied samples of wheat, rice, and flour contained both fortified and incurred EDB; corn bread mix, baby cereal, and bread contained only fortified EDB. The whole grains and intermediates were analyzed by the same basic procedural steps as in the official method for multifumigants: They were extracted by soaking in acetone-water (5 + 1). The baby cereal and bread were analyzed by a modification of the Rains and Holder hexane co-distillation procedure. EDB was determined by electron capture gas chromatography operated with an SP-1000 column. All products contained 3 different levels of EDB and were analyzed as blind duplicates. Overall mean recoveries ranged from 85.2% for 69.6 ppb to 105.0% for 4.35 ppb, both in baby cereal. Interlaboratory relative standard deviations ranged from 5.7% for 869 ppb in wheat to 20.2% for 69.6 ppb in baby cereal, both fortified. Mean levels of incurred EDB in wheat, rice, and flour were 926.7, 982.0, and 49.9 ppb, respectively; corresponding relative standard deviations were 9.9, 7.7, and 13.1%. The method was adopted official first action.     

Determination of rutin, catechin, epicatechin, and epicatechin gallate in buckwheat Fagopyrum esculentum Moench by micro-high-performance liquid chromatography with electrochemical detection

A simple and sensitive method has been developed for determining rutin, catechin, epicatechin, and epicatechin gallate in buckwheat (Fagopyrum esculentum Moench) flour and seeds by micro-high-performance liquid chromatography with electrochemical detection. Chromatography was performed using an octadecylsilica column, acetonitrile-water-formic acid (13:87:1, v/v/v) as a mobile phase, and an applied potential at +0.5 V vs Ag/AgCl. We found that Japanese buckwheat flour contains rutin (12.7 mg/100 g), catechin (3.30 mg/100 g), epicatechin (20.5 mg/100 g), and epicatechin gallate (1.27 mg/100 g). The relative standard deviations for rutin, catechin, epicatechin, and epicatechin gallate peak heights were less than 0.86% (n = 5). The detection limit of rutin was 0.86 ng/mL. Moreover, the present method was applied to the distribution analysis of these compounds in buckwheat seed. The embryo proper and cotyledons of a mature buckwheat seed contained rutin with the highest concentration as compared to other parts. This method is useful in determining rutin, catechin, epicatechin, and epicatechin gallate in buckwheat with a small amount of sample for quality control in the food industry.     

Improved liquid chromatography methods for the separation and quantification of biotin in NIST standard reference material 3280: multivitamin/multielement tablets

Two independently developed liquid chromatography (LC) methods for the quantitative determination of biotin in multivitamin/multielement tablets (NIST Standard Reference Material 3280 (SRM 3280)) are described. The methods use distinctly different tablet extraction solvents (methanol vs 1.5% aqueous formic acid) and analyte detection principles (mass spectrometry (MS) versus evaporative light-scattering detection (ELSD)) to ensure quantitative reliability. The use of different extraction and detection procedures allows cross-validation of the methods and enhances confidence in the final quantitative results. Both methods yield highly comparable results for the mean level of biotin (LC/MS = 26.5 mg/kg +/- 0.3 mg/kg (n = 12); LC/ELSD = 24.7 mg/kg +/- 1.7 mg/kg (n = 12)) in SRM 3280, yet the methods differ considerably in their analytical characteristics. The isotope-dilution LC/MS method exhibits excellent linearity from 0.02 ng to 77 ng biotin on-column with a method limit of detection (LOD) and limit of quantification (LOQ) of 0.02 ng (S/N > 3) and 0.06 ng (S/N > 10) biotin on-column, respectively. The LC/ELSD method exhibits good linearity from 155 ng to 9900 ng biotin on-column with a method LOD and LOQ of 155 ng (S/N > 3) and 310 ng (S/N > 10) biotin on-column, respectively. Method performance data indicates that the LC/MS method is analytically superior to the LC/ELSD method; however, either method in combination with SRM 3280 should provide quality assurance, accuracy, and traceability for biotin levels in multivitamin/multielement dietary supplements.     

High pressure liquid chromatographic determination of zearalenone in chicken tissues

A method is reported for the extraction and analysis of zearalenone in chicken fat, heart muscle, and kidney tissue by using high pressure liquid chromatography (HPLC). Zearalenone is extracted with acetonitrile, cleaned up with hexane, and extracted further with ethyl acetate. Zearalenone is determined by HPLC using a reverse phase radial compression separation system, an ultraviolet absorbance detector, and a mobile phase of acetonitrile-water (60 + 40) (v/v). Recoveries of zearalenone added at levels from 50 to 200 ng/g are in the range 82.6-95.1%.     

Determination of albendazole and its major metabolites in the muscle tissues of Atlantic salmon,tilapia, and rainbow trout by high performance liquid chromatography with fluorometric detection

A liquid chromatographic procedure for the determination of albendazole ([5-(propylthio)-1H-benzimidazol-2yl]carbamic acid methyl ester) and its major metabolites, albendazole sulfoxide, albendazole sulfone, and albendazole-2- aminosulfone in rainbow trout, tilapia, and salmon muscle with adhering skin tissue is described. The muscle tissue samples are made alkaline with potassium carbonate and extracted with ethyl acetate. The extracts are further subjected to cleanup by utilizing a number of liquid-liquid extraction steps. After solvent evaporation, the residue is reconstituted in mobile phase and chromatographed. The chromatography is carried out on a reversed phase Luna C(18) column, using acetonitrile/methanol/buffer as a mobile phase and a fluorescence detector. The average recoveries from the fortified muscle tissue of the three fish species for albendazole (25-100 ppb), albendazole sulfoxide (15.5-62 ppb), albendazole sulfone (1-10 ppb), and albendazole-2- aminosulfone (10-100 ppb) were 94, 77, 82, and 67%, respectively. The average CV for each compound was < or =10%. The procedure was validated and then applied to the determination of albendazole and its three major metabolites in the muscle tissue of the three fish species obtained after orally dosing with albendazole.     

Plant Alkaline Fusion Technique Followed by Colorimetric Procedure for the Detection and Quantification of Total Silicon in Ornamental Plants

Silicon (Si)–determination procedures currently available require expensive equipment and must be modified to assess Si concentrations in plant tissues. A Si-determination procedure referred to as the plant alkaline fusion technique, or PAFT, was developed to assess total Si concentrations, specifically in plant tissue. The procedure consists of dry-ashing the plant material, alkaline fusion, solubilization of the fusion cake, dilution, and colorimetric determination to quantify total Si content. The fusion technique for solubilizing plant Si can be performed using sodium hydroxide (NaOH), nickel crucibles, and Bunsen burners. Silicon concentrations of two National Institute of Standards and Technology (NIST) standard reference materials (SRM) [pine needles (SRM 1575) and peach leaves (SRM 1547)], a rice straw standard (LSU#5), an NIST soil standard (SRM 2709), and five ornamental plant species were all assessed using the PAFT procedure, and then these values were compared to two different inductively coupled plasma–optical emission spectroscopy (ICP-OES) procedures conducted by independent laboratories. The PAFT Si determination procedure typically reported the greatest value or was within 15% of the two ICP-OES procedures while costing significantly less than both ICP-OES procedures.     

基质固相分散萃取-高效液相色谱串联质谱法测定土壤中残留的磺酰脲类除草剂

建立了基质固相分散萃取-高效液相色谱串联质谱法(MSPD-HPLC-MS/MS)测定土壤中3种磺酰脲类除草剂(氯磺隆、甲磺隆、苯磺隆)残留的分析方法。对基于球磨的基质固相分散萃取条件进行了详细优化,最终确定最佳条件为:0.2 g土壤样品、0.8 g HC-C18粉末状分散剂与直径为8 mm的小钢珠一起球磨10 min后,转移至空的玻璃萃取小柱,用10 m L乙腈洗脱,氮气吹干后用甲醇定容至0.6 m L,再经0.22μm的滤膜抽滤后装入自动进样瓶中。用Syncronis C18反相色谱柱分离,以甲醇(A)~1‰甲酸溶液(B)为流动相进行梯度洗脱,选择反应监测(SRM)模式下进行检测。氯磺隆在20~200μg·kg~(-1),甲磺隆和苯磺隆在10~200μg·kg~(-1)范围内线性良好,相关系数r在0.997 9~0.999 5。土壤样品的平均加标回收率在84.7%~104.6%,相对标准偏差在4.5%~7.9%(n=5)。方法的检出限(S/N=3)0.32~0.68μg·kg~(-1)。该方法简单、效率高、干扰少、回收率高,满足土壤中除草剂的残留分析要求。