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 18,428 document(s) hit in 31,850,051 MEDLINE articles (0.00 seconds)

A liquid chromatographic (LC) method for the analysis of sulfamethazine (SMT) in complete swine and cattle feed was collaboratively studied. The method uses post-column derivatization with dimethylaminobenzaldehyde and detection at 450 nm. To 5g finely ground feed, extractant (0.2N HCl + 1.5% diethylamine in 25% methanol), and internal standard solutions are added, and the SMT is extracted by shaking for 1 h. Clarified extract (high-level sample extract diluted to a target concentration of ca 5.5 microg/mL) is chromatographed on a Cla reversed-phase LC column with acetonitrile-2% acetic acid (17 + 83) mobile phase. Sulfamerazine is used as an internal, or surrogate standard to correct for variable recovery of sulfamethazine from a variety of feed matrixes. Six Youden matched-pair samples were sent to 10 collaborators in Korea, Canada, and the United States. Label claims on the commercial feeds ranged from 0.0077 to 0.22% SMT. The SMT mean recovery as determined from the 5 samples with known analyte content was 99.8%. The within-laboratory relative standard deviation (repeatability) ranged from 0.28 to 4.72%. Among-laboratory (including within-laboratory) relative standard deviation (reproducibility) ranged from 1.26 to 4.87%. The authors recommend the method for AOAC INTERNATIONAL Official First Action status.
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PMID:Determination of sulfamethazine in swine and cattle feed by reversed-phase liquid chromatography with post-column derivatization: collaborative study. 1077 62

The authors present a procedure of concurrent identification and quantification of amphetamine and metamphetamine in human hair. The method involves rinsing of the hair (distilled water 55 degrees C, 0.1 M hydrochloric acid, distilled water to neutral reaction, methanol) drying in air, homogenization by cutting (1-2 mm long), alkaline hydrolysis (20 mg hair, 1 ml 1 M sodium hydroxide, 55 degrees C, 120 min.), neutralization with 1 M hydrochloric acid to pH = 7, extracting benzoylation with 2,3,4,5,6-pentafluorobenzoyl chloride (0.3 ml 1 M sodium hydroxide, 4 ml cyclohexane, 30 ul cyclohexylamine in cyclohexane of a concentration of 20 ng/ul--internal standard, 50 ul aqueous solution of triethylamine hydrochloride concentration of 100 mg/ml--reaction catalyst and 10 ul of derivation agent 2,3,4,5,6-pentafluorobenzoyl chloride dilution 1:10, shaking for 5 mins. by hand and leaving to stand for 10 mins.), centrifugation (5 mins., 3000 rotations/min.), collection of 2 ml cyclohexane layer, its evaporation at 40 degrees C in nitrogen atmosphere and dilution with 100 ul cyclohexane. The derivated extract was subjected to analysis by the GC-MS method. The procedure was used for segmentation analysis of hair of two subjects abusing metamphetamine for prolonged periods. The revealed concentrations varied within the range of 0.99-5.25 mg/kg metamphetamine and 0.13-0.73 mg/kg amphetamine.
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PMID:[Determination of amphetamine and methamphetamine in human hair using gas chromatography/mass spectrometry]. 1091 34

A simple and reliable extraction method was developed for quantitative determination of both butyl- and phenyltin compounds in sediments by capillary gas chromatography combined with inductively coupled plasma mass spectrometry (GC-ICP-MS). Both types of organotin compounds were extracted quantitatively from sediment by mechanical shaking into tropolone-toluene and HCl-methanol. After phase separation and pH adjustment, these organotins were ethylated with sodium tetraethylborate. The method was evaluated by analyzing PACS-2 and NIES No. 12 sediment certified reference materials. The dibutyltin (DBT; 1.14 +/- 0.02 micrograms g-1) and tributyltin (TBT; 1.01 +/- 0.04 micrograms g-1) values observed in PACS-2 sediment closely matched the certified values (DBT, 1.09 +/- 0.15; TBT, 0.98 +/- 0.13 microgram g-1 as tin). The monobutyltin (MBT) value was higher (0.62 +/- 0.02 microgram g-1) by more than two fold over the reference value (0.3 microgram g-1 as tin). The concentrations of TBT (0.18 +/- 0.04 microgram g-1) and triphenyltin (TPhT; 0.0099 +/- 0.002 microgram g-1) in the NIES No. 12 sediment were also in good agreement with the certified and reference values of TBT (0.19 +/- 0.03 microgram g-1 as compound) and TPhT (0.008 microgram g-1 as compound), respectively. Recoveries of TBT, tripentyltin (TPeT) and TPhT from spiked sediments were satisfactory (TBT, 102 +/- 3.4%; TPrT, 96 +/- 3.4%; TPhT, 99 +/- 8.5%). The detection limits as tin were in the range 0.23-0.48 ng g-1 for a 0.5 g sample size. It is also noteworthy that clean-up of the extract is not necessary because of the superior selectivity of ICP-MS detection. The present method was successfully applied to marine sediment samples.
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PMID:A quantitative extraction method for the determination of trace amounts of both butyl- and phenyltin compounds in sediments by gas chromatography-inductively coupled plasma mass spectrometry. 1107 May 44

A collaborative study was conducted to evaluate a liquid chromatography (LC) method for ochratoxin A using sequential phenyl silane and immunoaffinity column cleanup. The method was tested at 3 different levels of ochratoxin A in roasted coffee, which spanned the range of possible future European regulatory limits. The test portion was extracted with methanol and sodium bicarbonate by shaking for 30 min. The extract was filtered, centrifuged, and then cleaned up on a phenyl silane column before being eluted from the washed column with methanol-water. The eluate was diluted with phosphate-buffered saline (PBS) and applied to an ochratoxin A immunoaffinity column, which was washed with water. The ochratoxin A was eluted with methanol, the solvent was evaporated, and the residue was redissolved in injection solvent. After injection of this solution onto a reversed-phase LC apparatus, ochratoxin A was measured by fluorescence detection. Eight laboratory samples of low-level naturally contaminated roasted coffee and 2 laboratory samples of blank coffee (< 0.2 ng/g ochratoxin A at the signal-to-noise ratio of 3:1), along with ampules of ochratoxin A calibrant and spiking solutions, were sent to 15 laboratories in 13 different European countries. Test portions of the laboratory samples were spiked at levels of 4 ng/g ochratoxin A, and recoveries ranged from 65 to 97%. Based on results for spiked blank material (blind duplicates) and naturally contaminated material (blind duplicates at 3 levels), the relative standard deviation for repeatability (RSDr) ranged from 2 to 22% and the relative standard deviation for reproducibility (RSDR) ranged from 14 to 26%. The method showed acceptable within- and between-laboratory precision, as evidenced by HORRAT values, at the low level of determination for ochratoxin A in roasted coffee.
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PMID:Combined phenyl silane and immunoaffinity column cleanup with liquid chromatography for determination of ochratoxin A in roasted coffee: collaborative study. 1132 9

Sampling and analytical methods were developed for commonly used chloroacetanilide, chlorotriazine, and 2,4-D herbicides in hand washes, on dermal patches, and in air. Eight herbicides selected for study were alachlor, atrazine, cyanazine, 2,4-dichlorophenoxyacetic acid (2,4-D), metolachlor, simazine, and two esters of 2,4-D, the 2-butoxyethyl ester (2,4-D, BE) and the 2-ethylhexyl ester (2,4-D, EH). The hand-wash method consisted of shaking the worker's hand in 150 mL of isopropanol in a polyethylene bag for 30 seconds. The dermal-patch method entailed attaching a 10-cm x 10-cm x 0.6-cm polyurethane foam (PUF) patch to the worker for exposure; recovery of the herbicides was achieved by extraction with 40 mL of isopropanol. The air method involved sampling with an OVS-2 tube (which contained an 11-mm quartz fiber filter and two beds of XAD-2 resin) and recovery with 2 mL of 10:90 methanol:methyl t-butyl ether. Analysis of each of the three sample types was performed by gas chromatography with an electron-capture detector. Diazomethane in solution was employed to convert 2,4-D as the free acid to the methyl ester in each of the three methods for ease of gas chromatography. Silicic acid was added to sample solutions to quench excess diazomethane. Limits of detection for all eight herbicides were matrix-dependent and, generally, less than 1 microgram per sample for each matrix. Sampling and analytical methods met NIOSH evaluation criteria for all herbicides in hand-wash samples, for seven herbicides in air samples (all herbicides except cyanazine), and for six herbicides in dermal-patch samples (all herbicides except cyanazine and 2,4-D). Speciation of 2,4-D esters and simultaneous determination of 2,4-D acid were possible without losses of the esters or of other herbicides (acetanilides and triazines) being determined.
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PMID:Development of sampling and analytical methods for concerted determination of commonly used chloroacetanilide, chlorotriazine, and 2,4-D herbicides in hand-wash, dermal-patch, and air samples. 1141 20

A method of quantitative analysis of nonylphenol polyethoxylates (NPnEOs) and their biodegration products (NPE-BDPs) in sewage sludge, which is effective, economical, and applicable to a high performance liquid chromatography was developed and actual sludge samples collected from Japanese sewage treatment plants (STPs) were analyzed using the method to confirm its effectiveness. Soxhlet extraction showed better recovery in a spike and recovery test than shaking extraction. Among the four pretreatments for Soxhlet extraction tested, the condition in which samples were freeze-dried, ultrasonicated, and extracted with methanol showed the best recovery efficiency. Quantitative analysis of NPE-BDPs in STP sludge resulted in 6.1 microg/g, 4.3 microg/g, and 8. microg/g in average concentration for NPnEOs (n=1-3), NPnEOs (n=4-18), and nonylphenol ethoxycarboxylates (NPnECs (n=1-3)), respectively, and the values of concentration were 100-1000 times higher than those in effluent at Japan's STPs. The results implied importance of quantitation of NPE-BDPs in sewage sludge to assess the risk to the environment.
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PMID:Development of a routine analytical procedure for nonylphenol polyethyoxylates and their biodegradation products in sludge from sewage treatment plants. 1179 39

Different liquid-solid extraction techniques, including room-temperature leaching with mechanical shaking, ultrasonic, and microwave-assisted extractions, have been evaluated for the quantitative speciation of tin for mono-, di-, and tributyltin (MBT, DBT, and TBT, respectively) in PACS-2 and BCR-646 certified reference materials. A methanol-acetic acid mixture was used as the extractant reagent in all cases. For this purpose, a mixed spike containing 119Sn-enriched MBT (79.7 At%), 118Sn-enriched DBT (86.7 At%), and 119Sn-enriched TBT (83.1 At%), was synthesized, characterized, and used for isotope dilution analysis. The isotopic composition of the mixed spike was determined by gas chromatography/ICPMS after aqueous ethylation using sodium tetraethylborate, and the determination of the concentration of the different species in the spike was performed by means of reverse isotope-dilution analysis using natural MBT, DBT, and TBT standards. In the analysis of the certified sediments, the sample was spiked with the mixed spike, extracted under different conditions, derivatized with sodium tetraethylborate, and extracted into hexane, and the isotope ratios 120/118 and 120/119 were measured as peak area ratios for all butyltin species after GC/ICPMS. Mass bias was corrected using a derivatized natural standard every three sample injections. Sequential degradation reactions during extraction (from TBT to DBT, from DBT to MBT, and from MBT to inorganic tin) were assumed, and mathematical equations were developed that allowed the determination of the correct species concentration and the decomposition factor for each of the transformation reactions. For ultrasonic extraction and mechanical shaking, negligible degradation reactions were observed. However, for microwave assisted extractions, degradation factors up to 7% (TBT to DBT) and 16% (DBT to MBT) were obtained for both reference materials when high-MW energy was applied in the extraction step. For the three extraction techniques tested, the DBT and TBT concentration values obtained for PACS-2 closely matched the certified values. However, for MBT the concentrations found by microwave and ultrasonic extraction were much higher than the certified value. This was not the case for mechanical shaking. The results obtained for BCR-646 using microwave assisted extraction were in good agreement with the certified values for all tin species.
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PMID:Evaluation of extraction techniques for the determination of butyltin compounds in sediments using isotope dilution-GC/ICPMS with 118Sn and 119Sn-enriched species. 1179 50

Three different calcareous soil samples from Lebanon were analyzed for total DDT pesticide residue using GC and ELISA methods. Two experiments were conducted on three different calcareous soil samples. In each experiment, triplicates of 5 gm soil samples were each fortified with standard solutions of DDE to reach concentrations of 0, 5, 25, 50, 100 and 200 ng g(-1) and allowed to equilibrate at room temperature for 6 hours. Each sample was then extracted with 25 mL of 90% methanol by shaking in glass bottles on a mechanical shaker for 16 hours. The bottles were allowed to stand for 30 minutes and aliquots were taken from the clear supernatant for analyses without further cleanup. The total DDT in the extract was measured in triplicate by GC and ELISA. The results indicated that the two methods were highly correlated (R = 0.955-0.994). Differences in soil properties did not affect the accuracy of the detection limits of ELISA. Immunoassay technique can be used for rapid and accurate measurement of total DDT residues in mineral calcareous soils in Lebanon.
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PMID:Comparison of gas chromatography and immunoassay methods for analysis of total DDT in calcareous soils. 1261 50

The objective was to evaluate the effect of sample preparation (pulverization under liquid nitrogen, homogenization, or sonication), time length of sonication (0-60 s), shaking in chloroform/methanol solvent (0, 2, 4, or 12 h), incubation in chloroform (0 or 12 h), and drying of extracted lipids at 50 degrees C (2, 4, 6, or 24 h), and sample size (50-250 mg) on quantification of total lipids from bovine liver. Pulverization under liquid nitrogen yielded the lowest recovery. Sonication was least time-consuming for sample preparation. Precise estimates and the greatest recovery were obtained with 30 s of sonication, at least 2 h of shaking in chloroform/methanol solvent, 12 h of incubation in chloroform, and at least 6 h of drying. Sample sizes of at least 150 mg gave precise estimates. The results demonstrate that sample preparation, time length of different steps of the extraction procedure, and sample size affect quantification of total lipid from bovine liver.
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PMID:Effect of sample preparation, length of time, and sample size on quantification of total lipids from bovine liver. 1267 Jan 42

Cultivation conditions affecting feather degradation by Bacillus sp. FK 46 were investigated. The results showed that feather was almost completely degraded under the following conditions: 1% whole chicken feather as a substrate at the initial medium pH of 9 with 5% bacterial inoculum, at a temperature of 37 degrees C and a shaking speed of 250 rev/min. Glucose, methanol, Tween 80 and Triton X-100, however, had no effect on feather degradation. After feather was degraded, its residue and fermented broth would become a protein feed for animals.
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PMID:Feather degradation by Bacillus sp. FK 46 in submerged cultivation. 1268 66


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