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1.
A method is described for the determination of pentachlorophenol (PCP) in gelatin. The method employs acid and heat to hydrolyze the gelatin matrix, a base partition and wash for separation and cleanup, and a reacidification and extraction with hexane for direct determination of PCP, without preparation of a derivative, using gas chromatography (GC) with a 1% SP- 124ODA liquid phase and a 63Ni electron capture detector. Recoveries averaged 106% for fortifications between 0.02 and 1.0 ppm. The limit of quantitation is 20 ppb. The limit of detection is 4-6 ppb. The method, which has undergone a successful intralaboratory trial, is simple and rapid, and requires only general laboratory reagents and equipment. GC of the acetate derivative of PCP is used for confirmation of identity.  相似文献   

2.
A gas chromatographic assay was developed to determine major residues of morantel in bovine milk over a range that is suitable for monitoring residues of the drug. The method is based on hydrolysis of the N-methyl-tetrahydropyrimidine portion of morantel and its metabolites to N-methyl-1,3-propanediamine, and converting the diamine to an N,N-bis-(2-nitro-4-trifluoromethylphenyl) derivative. The addition of an internal standard, the N-desmethyl-N-ethyl homolog of pyrantel, to the milk sample circumvents any potential problem that could arise from variable reaction yields, and eliminates the true recovery as a factor affecting the accuracy and precision of the procedure. The concentrations of the derivatives are determined by pulsed electron capture gas chromatography over a linear dynamic range that is equivalent to 12.5-50 ppb morantel. The method was evaluated at the 0, 12.5, 25, and 50 ppb levels in fortified bovine milk, and in a withdrawal sample containing physiologically incurred morantel residues. Mean values of 14 +/- 1.7, 24 +/- 3.7, and 47 +/- 6.9 were found for the fortified samples, approximately 3 ppb for control milk, and 16 +/- 1.7 ppb for the withdrawal sample.  相似文献   

3.
贾铮  肖志明  李兰  樊霞 《农业工程学报》2016,32(12):303-308
为了规范饲用酸化剂的使用和管理,建立一种快速、准确的多种有机酸同步检测方法应需而生。该文以实现饲料酸化剂中多种有机酸的同步检测为目标,基于离子排斥色谱技术,对饲料酸化剂中多种有机酸(柠檬酸、酒石酸、苹果酸、乳酸、甲酸、乙酸、富马酸、丙酸和丁酸)的检测条件进行了优化研究。研究采用Bio-Rad Aminex HPX-87H(300mm×7.8 mmΦ,9μm)离子排斥色谱柱及二极管阵列检测器,以硫酸溶液作为流动相,比较了不同流动相浓度、不同柱温、不同流动相流速、不同检测波长等色谱条件对同步检测饲料酸化剂中9中有机酸的影响;以上述优选的条件建立分析方法,考察此方法的线性范围和检出限、回收率和精密度,并用实际样品进行了验证。研究结果表明:以0.025 mol/L硫酸溶液为流动相,流速0.70 m L/min,柱温30℃,DAD检测波长为210 nm,以保留时间结合待测物质的紫外特征吸收光谱进行定性分析,外标法进行定量分析。9种有机酸组分的质量浓度与其峰面积在一定范围内呈良好线性关系,决定系数0.999,9种有机酸组分在20 min内可以得到良好分离;方法检出限为0.01~2.4 mg/L,加标回收率为90.7%~101.1%,相对标准偏差为0.91%~3.33%。基于上述条件建立的检测方法能够满足饲料酸化剂中多种有机酸成分的同步定量分析。  相似文献   

4.
Liquid chromatography with electrochemical detector (LC-ED), using a chemically modified electrode coated with a metalloporphyrin film, is reported for determination of bisphenol A (BPA) migration from polycarbonate baby bottles. The extraction process of the samples was performed according to regulations of the Southern Common Market (MERCOSUR), where certain food-simulating liquids [(A) distilled water, (B) acetic acid 3% V/V in distilled water, and (C) ethanol 15% V/V in distilled water] are defined along with controlled time and temperature conditions. The baseline obtained using the naked electrode showed a considerable drift which increased the detection limit. This effect was suppressed with the chemically modified electrode. A linear range up to 450 ppb along with a detection limit of 20 ppb for the amperometric detection technique was observed. The procedure described herein allowed lowering the detection limit of the method to 0.2 ppb. The value found for BPA in the food-simulating liquid is 1.2 ppb, which is below the tolerance limit for specific migration (4.8 ppm).  相似文献   

5.
Deuterated acetyl derivatives (3-trideutero-acetyl-T-2 and 15-trideutero-HT-2) were prepared for use as internal standards for the quantitation of T-2 and HT-2 in blood by tandem mass spectrometry. The method used was multiple reaction monitoring (MRM), which essentially involves the selection of a parent ion for analysis followed by monitoring of the daughter ions generated by collision activated decomposition. The parent ions chosen for the trifluoroacetate derivative of T-2 and HT-2 were m/z+ 478 and 532, respectively. Both parents yield the same daughter ions, i.e., 180, 138, and 121. HT-2 and T-2 were added to blood extracts in amounts ranging from 1 to 20 ppb. The limit of detection is about 0.5 ppb with an effective detection limit of 1.0 ppb in a range of 1-20 ppb. The recovery is about 90%. This method can be used by veterinarians for purposes of diagnostics. It can be used for urine as well as blood.  相似文献   

6.
The present paper describes a method for determination of oxolinic acid in salmon muscle tissue. Tissue (0.5-2 g) mixed with 2 g anhydrous sodium sulfate is extracted twice with ethyl acetate, centrifuged, and the extract evaporated. The residue is partitioned in a mixture of hexane and 0.01M oxalic acid and the aqueous phase chromatographed using fluorescence detection at 327 nm excitation and 369 nm emission. Calibration and standard curves are linear from 10-200 ppb and 100-2000 ppb at different sensitivity settings. Recoveries ranged from 71-83% in spiked blanks, with a CV of 4-10.3% over a 2-week period. Preliminary results in treated salmon were variable, possibly because some fish refused to eat medicated feed.  相似文献   

7.
A new cleanup procedure is described for chlorinated hydrocarbon residues in butterfat. The method is based on the dropwise addition of H2SO4 to a fat solution column and continuous removal of the lipids and the acid. The cleanup of 0.25-2.0 g fat requires only 10-40 ml sulfuric acid and 12-17 ml petroleum ether. There is no need for any further cleanup step, solvent evaporation, or centrifugation. The method is easy to standardize and is suitable for automation. At least 30 fat samples can be cleaned up manually by one analyst in one day. Recoveries were complete (greater than 90%) for polychlorinated biphenyl compounds and for 13 chlorinated pesticides of 16 examined. The method was tested on chlorinated hydrocarbon residues in commercial butter and the results were compared with those obtained with the acetonitrile method. The versatility and limitations of the method were investigated by varying the sulfuric acid strength, initial fat solution concentration, and column dimensions.  相似文献   

8.
A method is described for the gas-liquid chromatographic determination of traces of selenium in marine biological materials. The method is based on the reaction of Se(IV) with bromo- and chloro-substituted 1,2-diaminobenzenes. The benzoselenadiazoles so formed are sensitive to electron capture detection. The sample is digested in a nitric-perchloric acid mixture and selenium is reduced to the IV oxidation state. Different aliquots of the digest solution are reacted with either 4-bromo- or 4-chloro-1,2-diaminobenzene to quantitatively form the corresponding 2,1,3-benzoselenadiazole. Recovery of added selenite to a fish meal sample was 95% for the bromo derivative and 101% for the chloro derivative. Different portions of a well mixed fish meal sample were analyzed in independent laboratories by the fluorometric method and by atomic absorption spectrophotometry (hydride generation). The following mean values (microgram/g) were found: present method 1.89, fluorometric method 1.91, atomic absorption method 2.1. The lower limit of detection for the method described was 13 ng, using the bromo derivative, and 27 ng, using the chloro derivative.  相似文献   

9.
A liquid chromatographic method for the multiresidue determination of tetracyclines (TCs) in feeds is described. The levels of quantitation were 10 ppm each for tetracycline-HCl (TC), oxytetracycline (OTC), and chlortetracycline-HCl (CTC); the detection limit was 40 ppb for each. The calibration curves were linear between 2.5 and 100 ppm. The procedure involved double extraction with pH 2.0 and pH 4.5 McIlvain buffers, cleanup on a Sephadex LH-20 column, separation on a Nova-Pak C18 column, and detection at 370 nm. Recoveries of 10 micrograms/g of each TC in multiresidue feed samples ranged from 55.8 to 75.5% for OTC, 71.6 to 100% for TC, and 22.4 to 60.6% for CTC. The identities of the TCs were confirmed by thin layer chromatography.  相似文献   

10.
An analytical method was developed for determining benzo(a)pyrene in foods, suitable for routine use. The method consists of 4 cleanup steps: (1) alkali cleavage of sample, (2) preliminary silica gel column chromatography, (3) selective extraction with concentrated sulfuric acid, and (4) further silica gel column chromatography. Recoveries of benzo(a)pyrene added to 50 g (or 10 g) food at levels of 0.4 ppb (or 2 ppb) ranged from 70% for short-necked clam and mackeral to 85% for chicken meat. The sulfuric acid extraction step affords a simple method for isolating benzo(a)pyrene from various kinds of interfering substances which could not be separated by existing methods.  相似文献   

11.
A method for the accurate one-dimensional thin layer chromatographic (TLC) determination of aflatoxins B1, B2, G1, and G2 in mixed feeds is presented. The aflatoxins are extracted from the sample with chloroform and purified by solvent partitioning. Each aflatoxin is separated from pulp interference by thin layer chromatography on aluminum-backed silica plates. The separated aflatoxins are detected by fluorescence densitometry. Average recoveries for samples spiked from 10 to 100 ppb B1 and G1 and from 3 to 30 ppb B2 and G2 are 82, 84, 95, and 94% for B1, B2, G1, and G2, respectively. The above recovery data, when analyzed for overall method repeatability, produced relative standard deviations of 6.8, 4.3, 6.9, and 7.6% for B1, B2, G1, and G2, respectively. Minimum detection level is less than 1 ppb for each aflatoxin. B1 is confirmed by trifluoroacetic acid derivative formation on a silica TLC plate.  相似文献   

12.
A rapid and sensitive liquid chromatographic method for determination of total vitamin C in foods and beverages is described. Ascorbic acid and dehydroascorbic acid are extracted with sulfuric acid solution, and the dehydroascorbic acid in the extract is reduced to ascorbic acid by dithiothreitol at pH 7. The reduction is complete in 2 min at room temperature. The resulting total ascorbic acid is separated on an anion exclusion/high speed column with 20 mM sulfuric acid as eluant and detected amperometrically with a platinum electrode operating at +0.6-0.8 V vs Ag/AgCl reference electrode. Dithiothreitol (retention time, 3.2 min) does not interfere with the separation and detection of ascorbic acid (retention time, 1.3 min). The dehydroascorbic acid content can be estimated as the difference in ascorbic acid content measured with and without reduction by dithiothreitol. The completeness of the reduction was demonstrated by purposely allowing the oxidation of ascorbic acid in the food extract and determining the total vitamin C after reduction. The determinations of vitamin C content in selected foods and beverages were in good agreement with the expected values. Total analysis time for vitamin C is 10 min and the detection limit is 0.1 ng. The method is specific for vitamin C, and interference by other food constituents is minimal.  相似文献   

13.
An improved method has been developed for the determination of benzyl penicillin in animal tissues. Tissues are fortified with a known amount of penicillin V (internal standard) and extracted with water. The extract is deproteinized with sulfuric acid and sodium tungstate, filtered, and concentrated on a conditioned C18 solid phase extraction column. Penicillin V and benzyl penicillin are then eluted from the column with 1 mL 60% acetonitrile-35% water-5% 0.2M phosphate buffer solution and derivatized with 1 mL 1,2,4-triazole-mercuric chloride solution at 65 degrees C for 30 min. An aliquot of this sample is analyzed by reverse phase liquid chromatography with UV detection at 325 nm. The limit of detection is 5 micrograms/kg (ppb) penicillin G (8.4 IU/kg) in liver, kidney, and muscle tissues).  相似文献   

14.
A widely used method for analyzing hydrolyzable tannins afer reaction with KIO(3) has been modified to include a methanolysis step followed by oxidation with KIO(3). In the new method, hydrolyzable tannins (gallotannins and ellagitannins) are reacted at 85 degrees C for 20 h in methanol/sulfuric acid to quantitatively release methyl gallate. Dried plant samples can be methanolyzed under the same conditions to convert hydrolyzable tannins to methyl gallate. Oxidation of the methyl gallate by KIO(3) at pH 5.5, 30 degrees C, forms a chromophore with lambda(max) 525 nm, which is determined spectrophotometrically. The detection limit of the method is 1.5 microg of methyl gallate, and with plant samples, relative standard deviations of less than 3% were obtained.  相似文献   

15.
A method was developed that is suitable for screening eggs for a variety of nonpolar residues in a single procedure. Residues are extracted by silica solid-phase extraction (SPE). Analysis is conducted via reverse-phase gradient liquid chromatography, electrospray ionization, and tandem ion trap mass spectrometry. For screening purposes (based on a single precursor-product ion transition) the method can detect ionophore (lasalocid, monensin, salinomycin, narasin) and macrolide (erythromycin, tylosin) residues in egg at approximately 1 ng/mL (ppb) and above and novobiocin residues at approximately 3 ppb and above. Conditions are described for confirmatory analysis based on multiple ions in the product ion spectrum. The extraction efficiency for ionophores was estimated at 60-85%, depending on drug. Recovery of macrolides and novobiocin was not as good (estimated at 40-55% after a hexane wash of the final extract was included), but the method consistently screened and confirmed these residues at concentrations below the target of 10 ppb. The method was applied to eggs from hens dosed with each drug individually. Lasalocid was found to have the highest probability of detection in eggs based on its high ionization efficiency and higher rate of deposition relative to the other drugs. The method is part of a larger scheme to provide surveillance methods for a wide variety of drug residues in eggs.  相似文献   

16.
A method for the quantitative determination of fluoroacetate (FAC) residues in animal tissues is described. The procedure involves tungstic acid extraction, partitioning into ethyl acetate, evaporation of ethyl acetate, derivatization with pentafluorobenzyl bromide (PFB), and analysis of the resulting derivative (PFB-FAC) by capillary gas chromatography-mass spectrometry (CGC-MS) with specific ion monitoring (SIM). The tungstic acid system extracted 96.8 +/- 4.2% of the endogenous 14C-1080 residues in rat tissues. Recovery of FAC during the extraction, purification, and derivatization procedures is established by use of a 14C-FAC spike. 1,2-Dibromobenzene is used as an internal standard for the CGC-MS analysis. PFB-FAC is identified on the basis of comparative retention times and the relative intensities of m/z 257.9 and 181.0. PFB-FAC is quantitated by comparing the response at m/z 257.9 to a PFB-FAC standard curve. Routine sensitivity of the method allows determination of 10 ppb fluoroacetate in tissue.  相似文献   

17.
A gas-liquid chromatographic (GLC) method has been developed for the determination of the experimental herbicide 3,6-dichloropicolinic acid (Dowco 290) in soils. The method involves extraction of 1 g soil samples with 1N NaCl at approximately pH 7, methylation with diazomethane utilizing a microgenerator, and detection by electron capture GLC. Interferences are small, so that a cleanup step is not necessary even at the 6 ppb level. The procedure is rapid, requiring only 45 min/sample. Recoveries range from 84 to 94% at the 6-1000 ppb level with a minimum detectable limit of 6 ppb. Standard deviations for the percentage recovery values vary from 10.9 to 2.3 for the tested range of 6.7-670 ppb, respectively.  相似文献   

18.
A quantitative method is described for the measurement of N-mononitrosopiperazine (NPIP) and N,N'-dinitrosopiperazine (DNPIP) in drug formulations containing piperazine, using a gas chromatograph interfaced to a thermal energy analyzer (GC/TEA). The method has detection limits of 20 ppb for NPIP and 12 ppb for DNPIP. In a survey of 6 products available on the Canadian market, all contained NPIP at levels of 0.38-15.3 micrograms NPIP/g piperazine and none contained any detectable amount of DNPIP.  相似文献   

19.
Ethylene dibromide (EDB) levels in food samples were determined by gas chromatography with a high-resolution capillary column and electron capture detector. The capillary column used was 3 mm id X 25 m cross-linked 5% phenylmethyl silicone. Column temperature was set at 40 degrees C by a coolant containing carbon dioxide gas. Optimum temperatures of the injection port and detector were 200 and 350 degrees C, respectively. The detection limit was 0.5 ppb and linear from 1 to 20 pg on the dynamic range. EDB residues in food samples were extracted with n-hexane by steam distillation. A few impurity peaks appeared near EDB on the chromatogram; however, the EDB peak was resolved. Recoveries of EDB from wheat and brown rice ranged from 66.1 to 99.6%. EDB was detected in 3 samples of imported wheat at a range of 0.74-1.70 ppb, and was not detected at all in 37 samples. The EDB remaining in EDB-fortified cookies after baking was examined. The amounts of EDB were reduced to 30 to 50% of the original amounts by kneading the dough, and to below 1.5% by baking.  相似文献   

20.
A method has been developed for the extraction, cleanup, derivatization, detection, and quantitation of hexachlorophene (HCP) residues from 2 types of plant storage tissue high in lipid content. Wet soybean or peanut tissue was homogenized and extracted with ethyl ether and chromatographed on silica gel to remove the neutral lipids. The cleaned up sample was methylated with diazomethane and the dimethoxyhexachlorophene was eluted from a second silical gel column and chromatographed on a 6' glass column packed with 3% OV-1 or 3% SE-30 on Gas-Chrom Q. The instrument detection limit for the 63Ni electron capture detector was less than 0.1 ng for dimethoxyhexachlorophene and about 1 ppb HCP residue in plant issue. Recovery of 10-420 ppb HCP added to tissue averaged 90.9 +/- 5.7%. Interfering substances were removed, column life was increased, peak sharpness was increased, and tailing of the parent compound was decreased by using appropriate column chromatography.  相似文献   

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