首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 577 毫秒
1.
《Analytical letters》2012,45(11):1412-1425
Background: Lipid removal from biological samples can be achieved by addition of concentrated sulfuric acid. However, certain persistent organic pollutants (POPs) such as chlorophenols are decomposed by sulfuric acid treatment and, thus, a more gentle lipid reduction method is needed for extraction of many environmental contaminants from biological samples. Membrane dialysis extraction (MDE) is a non-disruptive method to extract POPs from biological matrices.

Methods: Human breast milk samples were spiked with radiolabelled p,p′-dichlorodiphenyl trichloroethane ([C-14]-DDT) as a POP proxy and extracted using solid phase extraction (SPE). The extracts obtained were dialyzed by MDE in low-density polyethylene tubings containing a mixture of n-hexane and dichloromethane for 24 h, 48 h, or 72 h.

Results: The lipid content was reduced by 86.2% after one dialysis cycle of 24 h using MDE, and 87.1% recovery of the [C-14]-DDT standard was obtained. The DDT recovery could be further increased up to 96.3% and 98.1% by repeating the dialyses for one or two more cycles, respectively. However, the increased [C-14]-DDT recovery includes a concomitant increase in lipid carryover from 13.8% with one dialysis cycle to 22.1% with three cycles.

Conclusion: An SPE procedure for extracting POPs from breast milk and dialytic conditions for isolation of the extracted POP with minimal lipid carryover was established. The method is nondestructive and acceptable recoveries can be obtained within a single solvent shift as demonstrated by spiking standards. The lipid carryover was minimized, and the method may be considered for lipid removal before HPLC or GC analysis of environmental contaminants.  相似文献   

2.
《Analytical letters》2012,45(12):2407-2423
ABSTRACT

A rapid and sensitive flow injection method is developed for the quantitation of glutamate in food samples. The method incorporates a covalently immobilized glutamate oxidase and peroxidase bioreactor linked in tandem. The H2O2 liberated from the glutamate samples as a result of enzymatic action is monitored spectrophotometrically at 552 nm using 4-aminoantipyrine and 3-dimethylaminobenzoic acid as a new chromogenic reagent. Glutamate calibration curves are linear up to 140 μM with a detection limit of 1 μM. Recovery yields from soup matrices are in the range 97 – 101%. Inter- and intra-day precision studies gave CV's of less than 3.5%. The immobilized enzymes show good storage and operational stabilities. Up to 40 samples h?1 can be manually analyzed. Excellent correlation is obtained from a comparison of the glutamate content of various soup brands and matrix type (solid, condensed and broths) obtained by the proposed FI method with those obtained for the same samples analyzed by the standard reference method (y 0.99x + 0.034).  相似文献   

3.
《Analytical letters》2012,45(2):457-467
Abstract

Polychlorinated biphenyls often occur simultaneously in environmental samples complicating the identification and quantification of chlordane. A method is presented for the separation of chlordane and two of its metabolites from several polychlorinated biphenyl mixtures. Soil samples were subjected to controlled environments so that degradation of PCB residues could be followed over a period of 10 months in order to examine interference to the method by PCB degradation products.  相似文献   

4.
Abstract

A method for integrating solid phase extraction of corticosteroids from biological samples with normal operation of reversed-phase HPLC is described. This method uses an extraction column mounted in place of the sample loop of a conventional injection valve to separate corticosteroids from some interfering compounds, and to effectively concentrate steroids from dilute samples. Both manual and fully automated chromatographs using this principle are described. A specific application to measurement of corticosterone in a rabbit serum preparation allows routine measurement of as little as 300 pg corticosterone per sample.  相似文献   

5.
Abstract

Shankhpushpi, traded in the Indian market is having different controversial botanical sources, that is, Convolvulus pluricaulis Choisy (Convulvulaceae), Clitoria ternatea Linn. (Papilionaceae), and Evolvulus alsinoides Linn. (Convulvulaceae). Simple, accurate and precise RP-HPLC-PDA method was established for quality assessment and discrimination of Shankhpushpi samples using chromatographic profiling method. In distinction to the routine method of quality assessment which uses single or dual marker peaks, all chromatographic data (retention times/variables) were used. Fifteen shankhpushpi samples were purchased from the market including authenticated samples of all three C. pluricaulis, C. ternatea, E. alsinoides. A total of 18 samples were analyzed by HPLC and the dataset was then treated with multivariate analyses like PCA and HCA by using MINITAB software. Thus, the developed method was useful in discriminating the Shankhpushpi samples and for the perseverance of quality control.  相似文献   

6.
Abstract

A high-performance liquid chromatographic method is described for the determination of chloroquine and its major metabolite desethylchloroquine in blood, plasma and urine. The procedure employs reversed-phase chromatography, with ultraviolet detection, and chlorpheniramine as an internal standard. One milliliter samples of biologic fluid are extracted in a single step with ether. The method has a sensitivity limit of 5 ng/ml for chloroquine and its metabolite. The applicability of the method is demonstrated by the analysis of blood and plasma samples obtained from rabbits following intravenous administration of chloroquine.  相似文献   

7.
Abstract

Low molecular weight carboxylic acids (C2-C8) were measured in aqueous samples using reverse phase HPLC coupled with conductivity detection. The aqueous samples are adjusted to pH 2 with H2SO4 and extracted with diethyl ether. The ether is allowed to evaporate over distilled water. The acid concentrate is analysed using a Zorbax-ODS column (25 mm × 4.6 mm). The method is simple, fast, and because of the selectivity of the conductivity detector, is relatively free from interferences. Average precision is estimated to be approximately ± 13% for the overall method.  相似文献   

8.
Abstract

We have measured the thermal conductivity in both solid and liquid states for two amorphous samples. The first is selenium doped with indium and the second is selenium doped with iodine. The concentration of In and I in the samples were 50000 ppm. Measurements were taken in a temperature range from 1000 to 370°C, and were carried out using the concentric cylinder method, which is based on the flow of heat through a cylindrical wall.  相似文献   

9.
《Analytical letters》2012,45(7):1791-1806
Abstract

The direct quantitative determination of phosphine in gaseous mixtures or in air samples is associated with a number of difficulties. the paper describes an alternative technique based on the oxidation of phosphine to phosphate. Phosphate can be analysed either by inductively coupled plasma-atomic emission spectrometry (ICP-AES) or by a colometric method.

Because the problem of a proper (quantitative) sampling of phosphine in the air of working environments and/or in gaseous mixtures is still unsolved, standard solutions of KH2PO4 have been used as analytes (“artifical samples”) in the ICP-AES method.

The statistics concerning the sample variances, obtained from the 2 methods mentioned above, indicate no differences.  相似文献   

10.
《Analytical letters》2012,45(14):1423-1433
Abstract

A sensitive method for the determination of caffeine in small plasma samples (50 μ1) is described. The samples are extracted with chloroform and the extrects are freed from interfering compounds by thin-layer chronatography. The spots of caffeine and the internal standard, 7-ethyl theophylline, are scraped off the plates and both compounds are eluted from the scrapings by means of a glass capillary collector. The caffeine in the eluate is quantitated by gas-  相似文献   

11.
《Analytical letters》2012,45(11):2195-2203
Abstract

A multi-target classification pattern recognition method based on the principal component analysis (PCA) has been proposed for computer-aided materials design considering the multiple specialties of materials. The designed sample with probable optimal specialties is determined in such way that its representing point should be at the optimal region in the PC sub-space, where most optimal samples can be discriminated from non-optimal samples by means of features. The experimental parameters of the sample represented by this point can be obtained using a non-linear inverse mapping method from the PC sub-space to the original space. Based on the information provided using the method, several samples of V-PTC materials with optimal multiple specialties are synthesized.  相似文献   

12.
《Analytical letters》2012,45(5):363-369
Abstract

Arsenic is determined in aqueous solutions produced from marine raw materials by atomic absorption spectrophotometry. Conversion of the aqueous extract to an ethanol-extract increases the sensitivity of determination by a factor of 4 to 5. The method is applied to some selected samples produced from marine raw materials.  相似文献   

13.
《Analytical letters》2012,45(11):1825-1835
Abstract

Protein concentration can be determined from its circular dichroism(CD) spectrum and from programs that calculate protein secondary structure content from CD. The method established was successfully applied to lysozyme and a de novo designed peptide with a standard error of about 5%, which is comparable to concentrations determined from an estimated extinction coefficient. This procedure is widely applicable in protein and peptide samples.  相似文献   

14.
《Analytical letters》2012,45(14):2244-2253
Abstract

This paper describes the application of the common and variation peak ratio dual-index sequence analysis methods to evaluate the quality of several tea samples obtained from different species and different areas based on 1HNMR fingerprint spectra (FPS). The method is able to determine the most similar sample groups and identify accurately the varieties and qualities of Blank tea, Longjing tea, and other green tea samples. Longjing tea is a famous brand of local green tea and has its own distinct characteristics. There were obvious differences between Uji tea from Japanese and Chinese green tea. The results showed that the dual index sequent analytical method provides a good approach to accurately describe the resemblance and differences among tea samples. It also can reflect tea's integrity and individual difference, and is an effective method to evaluate the quality of tea samples.  相似文献   

15.
《Analytical letters》2012,45(12):985-996
Abstract

An absolute method for the determination of trace amounts of sulfur in water and organic matrices is described. The method involves decomposition of organic samples in an oxygen bomb or oxidation of water samples with hydrogen peroxide. The resultant sulfates are reduced and distilled as hydrogen sulfide by the action of stannous phosphate in anhydrous phosphoric acid. The evolved hydrogen sulfide is absorbed in zinc acetate solution, converted to methylene blue and measured spectrophotometrically at 665 mm. The range is from 2 to 40 μg of sulfur using 1 cm cells.  相似文献   

16.
Abstract

A densitometric TLC method was developed for the quantification of allantoin in creams and suppositories used to treat vaginal infections. Allantoin was extracted with water at elevated temperature, diluted to a known volume, and separated by HP silica gel TLC. Allantoin was detected by spraying with p-dimethylamine-benzaldehyde reagent. The absorption of standards and samples was compared by in situ scanning. Recoveries of allantoin from authentic samples ranged from 96–102%, except for one sample that assayed high. The accuracy of the method was demonstrated by standard addition analysis of this sample.  相似文献   

17.
《Analytical letters》2012,45(12):941-949
Abstract

An HPLC method for analysis of atenolol in human plasma and urine is presented. Based on alkaline extraction, acid backextraction and reverse phase ion-pair chromatography this method is quite specific for atenolol. For a 0.5 ml plasma sample the sensitivity ranges from 20 ng/ml in fasted healthy volunteers to 50 ng/ml in various groups of patients. A sensitivity in urine of 1.0 mcg/ml was sufficient for all samples studied. As presented this method has been used in several clinical pharmacokinetic studies involving hundreds of samples.  相似文献   

18.
《Analytical letters》2012,45(4):1033-1043
Abstract

A rapid method is proposed for separation of iron(III) with Aliquat 336S as the stationary phase coated on silica gel column with citric acid buffered at pH 4,5 as mobile phase. the extracted iron is stripped from the column with different mineral acids and determined spectrophotracally as its complex with 1,10-phenanthroline, Iron was separated from chromium, molybdenum, titanium and nickel which are generally associated in steel samples. Similar separations of iron from lead, zinc, cadmium, bismuth and cobalt have significance in environmental sample analysis. the method is extended for analysis of iron from samples of sediment and sea-water.  相似文献   

19.
《Analytical letters》2012,45(11):2293-2304
ABSTRACT

Micellization is described as a successful media for simultaneous fluorimetric determination of perylene, pyrene and triphenylene in water samples by reducing interference between them. A multivariate method based on synchronous fluorescence scan to estimate perylene, pyrene and triphenylene in their mixture solution has been proposed. The method does not require solving of large amounts of data obtained from the whole spectrum of the samples, thus making the analysis simple and fast. The method gives the best result for perylene and satisfactory results for pyrene and triphenylene. Analysis of water samples of two different origins spiked with known amount of perylene, pyrene and triphenylene also gives satisfactory result. Presence of fluoranthene up to 1 μM does not interfere in the analysis.  相似文献   

20.
《Analytical letters》2012,45(3):197-210
Abstract

A method for quantitative determination of nitrazepam in human plasma in the range 5 - 100 ng/ml is presented.

Nitrazepam is extracted with benzene from plasma samples of 0.5 ml, methylated with methyl iodide and determined gas chromatographically with an electron capture detector of 63Ni-type.

Acid dissociation constants of nitrazepam are determined and the partition properties studied with benzene, methylene chloride and diethyl ether as organic phases.

The selectivity of the method with respect to the metabolites has been thoroughly studied.  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号