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1.
An analytical method was developed to quantitate polychlorinated and polybrominated biphenyls (PCBs and PBBs, respectively) in human serum. The method includes denaturation of the proteins in serum, extraction, adsorption chromatography, and gas chromatography with electron capture detection. The coefficients of variation for determining the in vivo bound PCBs and PBBs ranged from 11.7 to 29.8% and 7.1 to 14.0%, respectively. The method is capable of measuring 10 ng PCBs and PBBs/mL in 4 mL serum.  相似文献   

2.
As part of an epidemiology study, extraction methods and extract cleanup procedures were developed and validated for polychlorinated biphenyls (PCBs) and DDE, an ubiquitous metabolite of DDT, in human milk, blood serum, and infant formula. Studies included quantitative and reproducible recovery of total lipids, and reproducible and reasonably high recoveries of these chlorinated compounds from the human body fluids and infant formula, including levels of environmental health interest. An extensive quality control and assurance program was designed for use with these methods. Some validation work on serum was done using radiolabeled 14C-Aroclor 1254. Dilution assays were developed to permit use of a constant procedure, which should minimize variability in results. Methods are based on selected organic solvent extraction and column chromatographic cleanup techniques and quantitation by electron capture gas chromatography (EC/GC). Using these extensively researched extraction and cleanup methods, the limits of detection for GC measurements were 10.0 and 2.00 ppb for PCBs and DDE, respectively, in milk and 4.00 and 0.80 ppb in serum.  相似文献   

3.
A multiresidue method was developed for the simultaneous determination of low parts per billion (ppb) concentrations of the herbicides alachlor, metolachlor, atrazine, and simazine in water and soil using isotope dilution gas chromatography/mass spectrometry (GC/MS). Known amounts of 15N,13C-alachlor and 2H5-atrazine were added to each sample as internal standards. The samples were then prepared by a solid phase extraction with no further cleanup. A high resolution GC/low resolution MS system with data acquisition in selected ion monitoring mode was used to quantitate herbicides in the extract. The limit of detection was 0.05 ppb for water and 0.5 ppb for soil. Accuracy greater than 80% and precision better than 4% was demonstrated with spiked samples.  相似文献   

4.
Recently, semicarbazide has been found in food in jars sealed with cap liners that were manufactured using azodicarbonamide as a blowing agent. These reports raised the concern that the use of azodicarbonamide-an approved dough conditioner-may result in semicarbazide residues in bread. To answer this question, a method based upon the previously reported liquid chromatography/tandem mass spectrometry determination of the semicarbazone of o-nitrobenzaldehyde was utilized. The method adopted for this work includes an extensive cleanup and reaction with o-nitrobenzaldehyde at pH 3.5, rather than with the widely used 0.1 M HCl, to form the semicarbazone derivative. A stable isotope dilution assay was used to determine the free semicarbazide present in the bread products. Levels of semicarbazide ranged from 10 to 1200 ppb in commercial bread products with azodicarbonamide listed among their ingredients.  相似文献   

5.
Perchlorate has contaminated water sources throughout the United States but particularly in the arid Southwest, an area containing large numbers of people and few water sources. Recent studies have demonstrated that perchlorate is present in alfalfa and that perchlorate is secreted into the milk of cows. Studies in lactating cows have indicated that only a small portion of a perchlorate dose could be accounted for by elimination in milk, feces, or urine. It was hypothesized that the remainder of the perchlorate dose was excreted as chloride ion. The purpose of this study was to determine the fate and disposition of (36)Cl-perchlorate in lactating dairy goats. Two goats (60 kg) were each orally administered 3.5 mg (16.5 muCi) of (36)Cl-perchlorate, a dose selected to approximate environmental perchlorate exposure but that would allow for adequate detection of radioactive residues after a 72 h withdrawal period. Blood, milk, urine, and feces were collected incrementally until slaughter at 72 h. Total radioactive residue (TRR) and perchlorate concentrations were measured using radiochemical techniques and liquid chromatography mass spectrometry (LC-MS-MS). Peak blood levels of TRR occurred at 12 h ( approximately 195 ppb) postdose; peak levels of parent perchlorate, however, occurred after only 2 h, suggesting that perchlorate metabolism occurred rapidly in the rumen. The serum half-life of perchlorate was estimated to be 2.3 h. After 24 h, perchlorate was not detectable in blood serum but TRR remained elevated (160 ppb) through 72 h. Milk perchlorate levels peaked at 12 h (155 ppb) and were no longer detectable by 36 h, even though TRRs were readily detected through 72 h. Perchlorate was not detectable in skeletal muscle or liver at slaughter (72 h). Chlorite and chlorate were not detected in any matrix. The only radioactive residues observed were perchlorate and chloride ion. Bioavailability of perchlorate was poor in lactating goats, but the perchlorate that was absorbed intact was rapidly eliminated in milk and urine.  相似文献   

6.
A rapid liquid chromatographic (LC) method was developed for a sensitive determination of nitrite in cured meats, using ion-exclusion chromatographic separation and electrochemical detection (IEC-EC). The current AOAC colorimetric method requires 2 h shaking in a steam bath to eliminate interference from reducing compounds such as ascorbic acid. In the present method, nitrite was analyzed in the presence of ascorbic acid without interference, and the extraction time was reduced to 1 min. The extracted nitrite was determined by ion chromatography using anion-exclusion/HS column and amperometric detector equipped with platinum or glassy carbon electrode operating at +1.0 V vs Ag/AgCl reference electrode. The detection limit was 1 ppb as NO2-. The recoveries of 50 ppm nitrite added to frankfurter and meat stick were 103 and 99.6%, respectively, with relative standard deviations less than 4%. The high speed, sensitivity, and selectivity make the new method a useful alternative to the AOAC colorimetric method.  相似文献   

7.
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   

8.
A method developed for the determination of ethylene dibromide in table-ready foods has been modified and expanded to include 7 other volatile halocarbons and carbon disulfide. Samples are stirred with water and purged with nitrogen for 0.5 h in a water bath at 100 degrees C. The analytes collected on a duplex trap composed of Tenax TA and XAD-4 resin are eluted with hexane and determined by gas chromatography with electron capture detection or Hall electrolytic conductivity detection. Flame photometric detection in the sulfur mode is used to determine carbon disulfide. Thick-film, wide-bore capillary columns are used exclusively in both the determination and confirmation of the halogenated analytes. The higher levels of analytes are also confirmed by full scan gas chromatography mass spectrometry (GC/MS). Samples are analyzed for carbon disulfide, methylene chloride, chloroform, 1,2-dichloroethane, methyl chloroform, carbon tetrachloride, trichloroethylene, 1,2-dibromoethane, and tetrachloroethylene. Initially, 19 table-ready foods from the Food and Drug Administration's Total Diet Study were analyzed by this method. A limited survey of those food items exhibiting high levels of analytes was conducted. Samples exhibited levels up to 3300 ppb (methyl chloroform in Parmesan cheese). Recoveries of all 9 analytes from fortified samples ranged from 83 to 104%. Chromatograms from this purge and trap method are clean, enabling quantitation levels of low parts per billion and sub-parts per billion to be achieved for the halogenated analytes. The quantitation limit for carbon disulfide is 12 ppb. Two compounds found in drinking water were identified by GC/MS as bromodichloromethane and chlorodibromomethane. Drinking water from several cities was analyzed for these trihalomethanes as well as for bromoform. Levels of up to 17 ppb bromodichloromethane were found. Recoveries ranged from 96 to 103%.  相似文献   

9.
Liquid chromatographic determination of sulfamethazine in milk   总被引：1，自引：0，他引：1  
A simple, relatively rapid liquid chromatographic method has been developed for the determination of sulfamethazine (SMZ) in milk at levels in the low ppb range. The method is based on extracting SMZ from milk with chloroform, evaporating the chloroform, dissolving the residues in hexane, extracting into buffers, and chromatographing the buffer solution. The method has been shown to determine levels as low as 5 ppb reliably. Levels greater than or equal to 7 ppb have been confirmed by gas chromatography/mass spectrometry after derivatization of extracts from fortified, incurred, and shelf milk. Intralaboratory recoveries and percent coefficients of variation are satisfactory. Sulfadimethoxine and sulfaquinoxaline can also be determined by the method. Application of the method to other dairy products is being investigated.  相似文献   

10.
Two hundred seventeen tap water samples, from homes in 26 counties of eastern Kentucky, western West Virginia, southeastern Ohio, and northeastern Tennessee, USA, were analyzed for arsenic (As) by Hydride Generation AAS. Nearly half of the 179 samples from private wells had detectable arsenic, and, of these, 43% had 0.5–1.0 ppb, 34%, 1.1–3.0 ppb, 6%, 3.1–5.0 ppb, 11%, 5.1–10.0 ppb, and 6% had As far exceeding the new Maximum Contamination Level (MCL) of 10 ppb recently set by the U.S. Environmental Protection Agency (USEPA). Based on the National Research Council’s 2001 report to the USEPA, the lifetime risk of bladder and lung cancer from water arsenic exposure at 10 ppb is about one in 333 individuals, which is much higher than the standard of one in 10,000 individuals set for other carcinogens. Even at 5 ppb, the risk is 1 in 667, at 3 ppb, 1 in 1000, and at 1 ppb, 1 in 3100. The incidence of arsenic-related cancers and other diseases in this coal-mining region is high, and 57% of the well water samples tested in this study had levels over 1 ppb As. Since Central Appalachian families rely heavily on private wells, and the U.S. Federal 2006 compliance edict does not apply to private water sources, more extensive sampling and analysis of well water in the region, using the most sensitive methodology available, is recommended. A public awareness campaign and routine health screening for arsenic exposure is also recommended.  相似文献   

11.
A synchronous derivative spectrofluorometric method is described for the determination of the plant growth regulator, gibberellic acid (GA3). The method is based on the formation of a fluorogen in concentrated sulfuric acid. The reaction is carried out at 85% sulfuric acid and in aqueous medium. The common fluorometric method with a linear dynamic range of 137-400 ppb, and a detection limit of 48 ppb is described. The synchronous first and second derivative method has linear dynamic ranges between 7.6-40 ppb and 12-40 ppb, with detection limits of 3.5 and 6.7 ppb, respectively. The influence of reaction variables and of other plant growth regulators present, and the application to residues on oranges, lemons, and grapes, are also described.  相似文献   

12.
A method was developed and validated to determine 5-hydroxyflunixin in raw bovine milk using liquid chromatography tandem mass spectrometry (LC/MS/MS). The mean recovery and percentage coefficient of variation (%CV) of 35 determinations for 5-hydroxyflunixin was 101% (5% CV). The theoretical limit of detection was 0.2 ppb with a validated lower limit of quantitation of 1 ppb and an upper limit of 150 ppb. Accuracy, precision, linearity, specificity, ruggedness, and storage stability were demonstrated. A LC/MS/MS confirmatory method using the extraction steps of the determinative method was developed and validated for 5-hydroxyflunixin in milk from cattle. Briefly, the determinative and confirmatory methods were based on an initial solvent (acetone/ethyl acetate) precipitation/extraction of acidified whole milk. The solvent precipitation/extraction effectively removed incurred ((14)C) residues from milk samples. The organic extract was then purified by solid phase extraction (SPE) using a strong cation exchange cartridge (sulfonic acid). The final SPE-purified sample was analyzed using LC/MS/MS. The methods are rapid, sensitive, and selective and provide for the determination and confirmation of 5-hydroxyflunixin at the 1 and 2 ppb levels, respectively.  相似文献   

13.
A method based on gas chromatography with electron capture detection was developed for the determination of ethylene dibromide (EDB) extracted from flour products. The procedure relies on the organic extraction of flour/water mixtures and uses an internal standard, 1-bromo-3-chloropropane. Recoveries of EDB at 10 and 100 ppb were 80.1 +/- 2.8% (SD) and 84.4 +/- 4.3%, respectively; recovery of the internal standard at the working concentration 500 ppb was 98.3 +/- 6.7%. Calibration curves were linear over the range 5-400 ppb, with a mean overall coefficient of variation of less than 5%. The reliability of the procedure was assessed by using gas chromatography combined with mass spectrometry. Results are shown for determination of EDB in locally milled flour products.  相似文献   

14.
A single-chain anti-atrazine antibody fragment, scAb (single-chain Fv with a CK domain), was expressed in Escherichia coli, and monomeric and dimeric species were preferentially purified from periplasmic extracts by chromatography upon nickel chelate immunosorbent columns or by immunoaffinity purification using a constant domain (CK) tag. Recombinant monomeric and dimeric antibody fragments, Fab, and intact monoclonal antibodies were compared in assays by competition between free atrazine in solution and (a) immobilized atrazine-bovine serum albumin conjugate (indirect assay) or (b) atrazine-alkaline phosphatase (direct assay). Recombinant antibody fragments provided a lower detection limit than either Fab or intact monoclonal antibody in both assay formats. Monomeric fragments displayed a sensitivity of detection down to 0.1 ppb, compared to 1.0 ppb for dimeric fragments and the parental monoclonal.  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.
The efficacy of a combination of two enzyme-linked immunosorbent assay (ELISA) kits was examined for screening the toxic equivalent (TEQ) concentrations of dioxins in retail fish. The coplanar PCB-EIA system, which is a competitive immunoassay specific for polychlorinated biphenyl (PCB) 118, was tested as a screening method for mono- ortho PCBs. The Ah immunoassay (Ah-I), which is an ELISA-based aryl hydrocarbon receptor binding assay, was analyzed for its screening ability for non- ortho PCBs, polychlorinated dibenzo- p-dioxins (PCDDs), and dibenzofurans (PCDFs). Dilution and recovery tests using purified fish extracts revealed no major interference of the matrix in the PCB-EIA and suggested that the matrix effect was minimized in the Ah-I. Finally, the results for the fish samples ( n = 20) showed a strong correlation between this method and high-resolution gas chromatography coupled to high-resolution mass spectrometry for the determination of the TEQ concentrations of mono- ortho PCBs ( r = 0.99) and non- ortho PCBs and PCDD/Fs ( r = 0.97). These data indicate that our method is suitable for screening retail fish to determine the TEQ concentrations of dioxins.  相似文献   

17.
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   

18.
A procedure has been developed and validated for measuring the concentration of pentobarbital residues in dry, extruded animal feed in the range of 3-200 ng/g (ppb) with an estimated limit of quantitation of 2 ppb. The method was developed for surveillance purposes: to measure the concentration of euthanizing agent which might be present in feeds incorporating rendered products which themselves might include some fraction of euthanized animals. A previously published qualitative procedure was modified by adding isotopically labelled pentobarbital as an internal standard. Dry feed was ground and extracted with methanol. The extract was loaded on a mixed-mode (C-18, anion exchange) solid-phase extraction cartridge designed for barbiturate residues. Pentobarbital was eluted and derivatized for gas chromatography/mass spectrometry in positive ion chemical ionization mode. Quantitation was based on the ratio of dimethyl-pentobarbital MH+ (m/z 255) vs dimethyl-pentobarbital-d(5) (m/z 260) in standards and extracts. Accuracy ranged from 112% at 3 ppb to 96% at 200 ppb, with relative standard deviations ranging from 4% at 3 ppb to 2% at 200 ppb.  相似文献   

19.
A sensitive and accurate detection method is of great importance in monitoring fusaproliferin levels in foods and animal feeds and evaluating its potential hazard to human and animal health. Several methods have been developed to detect fusaproliferin in cereals and cereal-related products, including thin-layer chromatography, high-performance liquid chromatography, enzyme-linked immunosorbent assay, liquid chromatography-mass spectrometry (MS), gas chromatography (GC), and GC-MS. However, these detection methods either suffer from low sensitivity, need expensive instruments, or are susceptible to interfering substances in the sample matrix. The GC-flame ionization detector method developed herein is sensitive, reliable, and easy to use for detecting fusaproliferin in corn and corn-based samples. Its detection limits were 0.04 ng for standard trimethylsilyl-fusaproliferin and about 5 ppb for fusaproliferin in corn samples. The limits of quantitation of this method were 0.15 ng fusaproliferin/injection and 20 ppb of fusaproliferin in corn samples. The recovery rates of fusaproliferin from corn samples spiked with 200, 1000, and 5000 ppb standard fusaproliferin were 109, 85.7, and 98.9% on average. The repeatability of the method was acceptable when evaluated by the Horwitz equation. Of the tested corn samples, three out of five sweet corn and the three yellow corn samples were found to have low levels of fusaproliferin (9.4-45.3 ppb). A moldy corn sample had a fusaproliferin content of 297 ppb.  相似文献   

20.
A collaborative study of a method for the determination of sterigmatocystin in cheese was conducted by 10 laboratories. The study included control samples and samples spiked at levels of 5, 10, and 25 ppb, in coded blind pairs. Recoveries were 60.0, 90.7, and 59.3%, outliers excluded, for the respective levels. The mean reproducibilities, outliers excluded, were 81.97, 17.13, and 52.77%, respectively. Mean repeatabilities, outliers excluded, were 77.66, 17.13, and 46.40%, respectively. Results of this collaborative study indicate that the method, modified as described in this report, is applicable to the determination of sterigmatocystin in cheese at low levels (5-50 ppb) for the purpose of surveys. With regard to the difficulty with thin-layer chromatography in this study, it is recommended that a more satisfactory determinative step be developed. Recommendation for official first action status is deferred.  相似文献   

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