生物医学样品中路易氏剂代谢产物分析检测方法研究进展

综述生物医学样品中路易氏剂代谢产物分析方法的研究现状,主要总结了路易氏剂染毒生物医学样品中标志物、样品制备和仪器分析方法的研究进展。路易氏剂染毒生物标志物主要包括游离和加合代谢产物两种,分析过程主要是对选定的生物标志物进行巯基化衍生和富集纯化,之后采用气相色谱–质谱、液相色谱–质谱等仪器对目标物进行检测鉴定。     

Methods for the extraction of microplastics in complex solid,water and biota samples

The widespread distribution of plastics, their persistence and ability to act as a vector of toxic chemicals has rendered them concerning emergent pollutants. The quantification of these contaminants is highly relevant for the evaluation of anthropogenic impacts on aquatic and terrestrial ecosystems and dependent of the efficacy of methods to separate microplastics from environmental matrices. Little information is available about the microplastic extraction methods on complex samples – i.e. samples with multiple types of matrices. Herein, methods for the separation of microplastics from complex samples are summarized and discussed based on their advantages and drawbacks focused on a comparative analysis of their efficiency on organic matter removal, polymer recovery and preservation of plastic integrity. The efficiency on microplastic recovery and organic matter reduction, as well as the examination of the effects of treatments on plastics are closely linked to the density and digestion approaches selected, the polymer features and the environmental matrix analyzed. High-density salt solutions are more effective for density separation, while oxidative methods have recurrently shown better rates of organic matter reduction (particularly in vegetal-rich samples) and plastic recovery, with little impact on plastics, while 10 % KOH has been described as highly efficient in samples containing animal organic matter. This comparative analysis highlights the benefits and limitations of different approaches for the analysis of microplastics in complex samples which may be helpful for the optimization and harmonization of the methods.     

Comparison of PCR and ELISA methods for the detection of bovine leucosis in dried blood spots

PCR and ELISA methods for the detection of bovine leucosis in dried blood spots on porous membranes were compared. Dry samples were analyzed through real-time PCR, using several diagnostic test systems. Nineteen and 20 samples were identified as positive by PCR and ELISA, respectively. Fourteen of these samples were identified as positive by both methods. When using PCR and ELISA, 26 samples were identified as positive for leucosis, which amounted to 47% of the total number of tested samples. The results of the analysis of dried and native samples were in good agreement. The obtained results showed that whole blood sampling in the form of dried spots applied on membrane can be used as a convenient and reliable way to obtain dry samples of biological fluids with the purpose of screening herds for infectious diseases, in particular for bovine leucosis.     

Structure determination of aligned samples of membrane proteins by NMR spectroscopy

The paper briefly reviews the process of determining the structures of membrane proteins by NMR spectroscopy of aligned samples, describes the integration of recent developments in the interpretation of spectra of aligned proteins and illustrates the application of these methods to the trans-membrane helical domain of a protein. The emerging methods of interpreting the spectral parameters from aligned samples of isotopically labeled proteins provide opportunities for simultaneously assigning the spectra and determining the structures of the proteins, and also for comparing the results from solid-state NMR experiments on completely aligned samples with those of solution NMR experiments on weakly aligned samples.     

Recent methods for the determination of peroxide-based explosives

In the last few years, the need to determine peroxide-based explosives in solid samples and air samples has resulted in the development of a series of new analytical methods for triacetonetriperoxide (TATP, acetone peroxide) and hexamethylenetriperoxidediamine (HMTD). In this review, after a short introduction describing the state of the art in the field, these new analytical methods are critically discussed. Particular emphasis is placed on spectroscopic and mass spectrometric methods as well as on chromatographic techniques with selective detection schemes. The potential of these methods to analyse unknown solid samples that might contain one or more of the explosives and to analyse peroxide-based explosives in air is evaluated.     

Detection and determination of antimalarial drugs and their metabolites in body fluids

This review of methods for determining antimalarial drugs in biological fluids has focused on the various analytical techniques for the assay of chloroquine, quinine, amodiaquine, mefloquine, proguanil, pyrimethamine, sulphadoxine, primaquine and some of their metabolites. The methods for determining antimalarials and their metabolites in biological samples have changed rapidly during the last eight to ten years with the increased use of chromatographic techniques. Chloroquine is still the most used antimalarial drug, and various methods of different complexity exist for the determination of chloroquine and its metabolites in biological fluids. The pharmacokinetics of chloroquine and other antimalarials have been updated using these new methods. The various analytical techniques have been discussed, from simple colorimetric methods of intermediate selectivity and sensitivity to highly sophisticated, selective and sensitive chromatographic methods applied in a modern analytical laboratory. Knowledge concerning the method for a particular study is determined by the type of application and the facilities, equipment and personnel available. Often is it useful to apply various methods when conducting a clinical study in malaria-endemic areas. Field-adapted methods for the analysis of urine samples can be applied at the study site for screening, and corresponding blood samples can be preserved for subsequent analysis in the laboratory. Selecting samples for laboratory analysis is based on clinical, parasitological and field-assay data. The wide array of methods available for chloroquine permit carefully tailored approaches to acquire the necessary analytical information in clinical field studies concerning the use of this drug. The development of additional field-adapted and field-interfaced methods for other commonly used antimalarials will provide similar flexibility in field studies of these drugs.     

Determination of epichlorohydrin in water and sewage samples

The simple, quick and effective methods for the analysis of epichlorohydrin (ECH) in water and sewage samples with the use of gas chromatography have been presented. From among all the methods developed, the procedures for monitoring drinking-water quality and the methods which allow the determination of epichlorohydrin in sewage samples have been selected.

The limits of ECH detection have been determined by direct aqueous injection (DAI) into the chromatographic column and an analysis with the application of a flame ionization detector (FID), a mass spectrometry detector (MS), an electron capture detector (ECD) and atomic emission detection (AED) detectors. The method allows the determination of ECH in water samples at the concentration level of 0.1 mg l⁻¹. Moreover, the developed methods of water samples preparation for chromatographic analysis using the following extraction methods: headspace (HS), stripping with adsorption on solid phase, liquid–liquid extraction (LLE), solid phase extraction (SPE) and solid phase microextraction (SPME) have been evaluated. The limits of ECH detection for each procedure with the application of gas chromatography (GC) combined with various detectors have been determined and their statistical evaluation has been presented. The SPME method allowed us to determine ECH in water samples at the concentration levels of 1.0 ng l⁻¹.

The results of studies on the choice of the selective methods allowing ECH analysis in sewage samples have been demonstrated. The applied SPME method was found to be a quick and effective technique to determine micro trace amounts of ECH in samples containing high amounts of various organic compounds.     

Evaluation of the BAX system for detection of Salmonella in selected foods: collaborative study

A multilaboratory study was conducted to compare the automated BAX System to the standard cultural methods for detection of Salmonella in selected foods. Five food types--frankfurters, raw ground beef, mozzarella cheese, raw frozen tilapia fish, and orange juice--at 3 inoculation levels, were analyzed by each method. A sixth food type, raw ground chicken, was tested using 3 naturally contaminated lots. A total of 16 laboratories representing government and industry participated. In this study, 1386 samples were analyzed, of which 1188 were paired samples and 198 were unpaired samples. Of the 1188 paired samples, 461 were positive by both methods and 404 were negative by both methods. Thirty-seven samples were positive by the BAX System but negative by the standard reference method, and 11 samples were positive by standard cultural method and negative by the BAX System. Of the 198 unpaired samples, 106 were positive by the BAX System and 60 were positive by the standard cultural method. A Chi square analysis of each of the 6 food types, at the 3 inoculation levels tested, was performed. For all foods, the BAX System demonstrated results comparable to those of the standard reference methods based on the Chi square results.     

The colorimetric determination of phosphates in water at low P.P.M. levels by automatic discrete-sample analysis.

Two colorimetric methods based on the formation of molybdenum blue (the tin(II)and ascorbic acid methods) have been adapted for the routine automatic determination of phosphate in water samples. Repeatability and linearity of both methods in discrete-sample automatic analysis are satisfactory. Some water samples were analyzed by both methods to compare final analytical results. An analytical rate of 60 readings per hour can be obtained.     

金汞捕集冷原子吸收法测定生物样品中痕量汞的试样预处理方法比较

采用微波炉分解和湿法分解进行生物样品的预处理，结合高灵敏的金汞捕集冷原子吸收法测定了生物样品中的痕量汞。对采用不同分解方法获得的试样进行了空白值、精密度、加标回收，准确度及检出限等性能方面的试验和比较，方法成功地用于生物样品中痕量汞的测定。     

Latest achievements in the analytical chemistry of actinides

New methods for separation and determination of actinides, widely used in analysis of actinides in technological and environmental samples are reviewed. Special attention is paid to obtaining and stabilizing transplutonium elements. (TPE) in extreme oxidation states. Their use in analytical practice resulted in expanding possibilities of methods for separation and determination of TPE. Solvent extraction, sorption and extraction chromatography are the basic methods for separation of TPE. Solvent extraction, sorption and extraction chromatography are the basic methods for separation of TPE. Methods of separation in gas phase and some other methods such as precipitation and coprecipitation are applied, however, to a lesser degree. Trends of development of these methods including those of various types of membrane extraction that succeeded in separation of TPE in both trivalent and other valence states have been shown. Attention is paid mainly to consideration of modern methods for determination of actinides, special distinction of such methods being low limits of determination, high precision and selectivity. Alpha- and beta-spectrometric methods with semiconductor detectors are the most advanced among various methods based on registration of nuclear radiation. Tremendous success has been achieved in development of emission-spectrometric methods for determination of trace amounts of actinides and various impure elements occurring in samples of actinides. Sensitive mass-spectrometric methods are widely used for determination of both isotope composition and content of elements in various samples including those which are highly radioactive. More simple and precise titrimetric methods based on using oxidizing-reducing or complexing agents are developed successfully. A large number of coulometric methods for determination of americium and berkelium, characterizing high precision and selectivity as well as luminescence methods have been developed.     

Quantitative validation of different protein precipitation methods in proteome analysis of blood platelets

For the preparation of proteins for proteome analysis, precipitation is frequently used to concentrate proteins and to remove interfering compounds. Various methods for protein precipitation are applied, which rely on different chemical principles. This study compares the changes in the protein composition of human blood platelet extracts after precipitation with ethanol (EtOH) or trichloroacetic acid (TCA). Both methods yielded the same amount of proteins from the platelet preparations. However, the EtOH-precipitated samples had to be dialyzed because of the considerable salt content. To characterize single platelet proteins, samples were analyzed by two-dimensional fluorescence differential gel electrophoresis. More than 90% of all the spots were equally present in the EtOH- and TCA-precipitated samples. However, both precipitation methods showed a smaller correlation with nonprecipitated samples (EtOH 74.9%, TCA 79.2%). Several proteins were either reduced or relatively enriched in the precipitated samples. The proteins varied randomly in molecular weight and isoelectric point. This study shows that protein precipitation leads to specific changes in the protein composition of proteomics samples. This depends more on the specific structure of the protein than on the precipitating agent used in the experiment.     

Separation,Preconcentration and Spectrophotometric Determination of Rhodamine B in Industrial,Cosmetic and Water Samples by Cloud Point and Solid Phase Extraction

The aim of this study is extraction, preconcentration and spectrophotometric determination of Rhodamine B (RB) in aqueous media by developing solid phase extraction (SPE) and cloud point extraction (CPE) methods. Amberlite XAD-1180 adsorbent and Tergitol NP-7 surfactant were used for SPE and CPE, respectively. Parameters of SPE and CPE which effected quantitative extractions were investigated and optimized. Matrix effects of some ions and dyes were analyzed at the optimum conditions. Developed methods were used to determine RB contents of anti-freeze, lipstick and water samples. The results of both methods demonstrated that the RB was quantitatively extracted and determined. RB contents of solid samples were found between 473 ± 15 and 317 ± 8 μg/g; 472 ± 11 and 312 ± 6 μg/L dye contents were determined for liquid samples. The methods were tested by analysis of spiked samples. Analytical characteristics of the methods were compared with each other and previously reported studies.     

Validation and Comparative Studies of Four Sulfonamide Immunoassays Based on the Same Generic Polyclonal Antibody

Four different immunoassays based on the same generic polyclonal antibody were validated by high performance liquid chromatography, respectively. They also were compared with each other in terms of sensitivity, precision, and accuracy for the quantification or screening of sulfonamide residues in food samples. Correlation studies showed that there was a good correlation between the immunoassays and liquid chromatography data. The conventional plate assay has better precision and the plate-enhanced chemiluminescent assay has higher sensitivity. These two methods all could be used as quantification methods for large numbers of samples and complements of the conventional analytical methods in laboratory. The flow-through strip assay has higher sensitivity and the dip-stick strip assay was less affected by matrix effect. These two methods all could be used as valuable tools for the rapid on-site screening of sulfonamide residues in animal-derived food samples.     

Surface area of antimony oxide by isotope exchange and other methods

Specific surface area of antimony oxide samples, one commercial and the other prepared from antimony trichloride have been measured by heterogeneous isotope exchange, gas adsorption, airpermeability and microscopic methods. Specific surface areas obtained by these four methods for the two samples were compared and the observed differences are explained.     

Diagnosis of lung cancer based on metal contents in serum and hair using multivariate statistical methods

The classification of normal and cancer groups with four multivariate methods according to metal contents in serum and hair samples has been discussed in the present paper. Results show that the four multivariate methods, stepwise discrimination analysis, principal components analysis, hierarchical cluster analysis, and stepwise cluster analysis can distinguish the two groups correctly. The independent samples of both normal and cancer groups were tested and can be distinguished correctly by the four methods. Therefore, these methods can be used as an aid for diagnosis of lung cancer according to the metal contents in serum and hair samples.     

Suppression of multiple scattering by photon cross-correlation techniques

The effectiveness of cross-correlation schemes for suppressing multiple scattering in light scattering measurements has been demonstrated convincingly. Thus, measurements on turbid samples can be analysed as though the samples were transparent, i.e. exhibiting only single scattering. The methods are now being used for new research, particularly in the study of concentrated colloidal dispersions. This article reviews the current state of the field with emphasis on the two-colour and three-dimensional dynamic light scattering techniques. Although these methods were originally designed to suppress multiple scattering in dynamic light scattering, it has recently been recognised that they are also effective in static light scattering. The cross-correlation schemes are compared briefly with other light-scattering methods for studying turbid and opaque samples such as fibre-optic probes and diffusing wave spectroscopy.     

Quantitative photoluminescence of broad band absorbing melanins: a procedure to correct for inner filter and re-absorption effects

We report methods for correcting the photoluminescence emission and excitation spectra of highly absorbing samples for re-absorption and inner filter effects. We derive the general form of the correction, and investigate various methods for determining the parameters. Additionally, the correction methods are tested with highly absorbing fluorescein and melanin (broadband absorption) solutions; the expected linear relationships between absorption and emission are recovered upon application of the correction, indicating that the methods are valid. These procedures allow accurate quantitative analysis of the emission of low quantum yield samples (such as melanin) at concentrations where absorption is significant.     

Radioisotope x-ray fluorescence analysis of ancient pottery from Tel Kouzama site in Damascus, Syria

The radioisotope X-ray fluorescence method has been utilized in the analysis of thirty nine archaeological pottery fragment samples from Tel Kouzama site, Damascus city, Syria. The samples were irradiated by a 109Cd radioisotope source (-9 10(8) Bq) for 1000 s. 17 chemical elements were determined. These elemental concentrations have been processed using two multivariate statistical methods, cluster and factor analysis in order to determine similarities and correlation between the various samples. Factor analysis confirms that samples were correctly classified by cluster analysis. These two methods suggest that samples can be considered to be manufactured using four different sources of raw material.