Validation study of the VitaKit A test kit for the determination of vitamin A in fluid milk (2% fat) for routine quality control. Performance Tested Method 061001

A validation study of VitaKit A for quantitation of total vitamin A in 2% fluid milk was carried out according to the guidelines provided by AOAC INTERNATIONAL. The VitaKit A was compared, in terms of repeatability and accuracy, with the U.S. Food and Drug Administration-Interstate Milk Shippers HPLC reference method for determination of total vitamin A in fluid milk with 2% fat. The data obtained by the VitaKit A method are in excellent agreement with the data obtained by the HPLC reference method. Further, a low LOD (0.33 international unit/mL) was obtained for the VitaKit A method; the presence of interferents, like cholesterol and vitamin D3, in the milk had minor influence on the quantitation of total vitamin A by the VitaKit A method. The VitaKit A test kit was found to be stable for 1 year from the date of manufacture when stored at 2-8 degrees C. The method requires 2 h processing time, compared to 1-2 days for the HPLC reference method. The results of this validation study clearly demonstrate that the VitaKit A method is reliable, rapid, and accurate for the quantitation of total vitamin A in fluid milk containing 2% milk fat. An independent study by Q Laboratories Inc., Cincinnati, OH, under the validation guidelines of AOAC INTERNATIONAL, confirmed these findings.     

On the calculation of the activation energy for solid state reactions

A novel and convenient method for the determination of the activation energy from isothermal kinetic runs has been proposed recently. A significant limitation of this method is discussed and is illustrated with an experimental example. A modification of the proposed method is suggested to circumvent this limitation.     

Organo-Laponites as novel mesoporous supports for manganese(III) salen catalysts

A Mn(III) salen complex was immobilized onto the Laponite surface using three different methodologies: method A, direct immobilization of the complex on the parent Laponite; method B, covalent anchoring through cyanuric chloride (CC); and method C, covalent anchoring through CC into a 3-aminopropyl)triethoxysilane (APTES) modified Laponite. All of the materials were characterized by FTIR, XPS, thermogravimetry, XRD, and nitrogen isotherms at 77 K, to gather information on the modifications introduced by the organo spacers within the Laponite surface, as well as on the anchored complex integrity; the Mn based materials were screened in the heterogeneous epoxidation of styrene. The results have shown that the immobilization of the manganese(III) salen complex by methods B and C have occurred at the edges of the clay particles through the spacers (APTES and CC) that have been anchored onto the Si-OH groups, whereas in method A, the complex is distributed throughout the clay surface, including the interlayer region. Therefore, the manganese loadings on the Laponites were as follows: materials prepared by method A > method B > method C. All of the heterogeneous catalysts showed high styrene epoxide selectivity, with that prepared by method A showing comparable styrene epoxide selectivity as the homogeneous phase reaction. The styrene epoxide yields decrease in the following order: materials prepared by method A > method B > method C (1st cycles), which parallel the respective support catalytic activity and decreasing of manganese content. The heterogeneous catalysts prepared using methods B and C could be reused at least for four times, with the former exhibiting the most stable catalytic activity, but that prepared by method A showed a significant decrease after two catalytic cycles.     

A data treatment method for detecting fluorescence anisotropy peaks in capillary electropherograms

A data treatment method is presented to detect fluorescence anisotropy (FA) peaks in capillary electrophoresis electropherograms. The data treatment method converts plots of fluorescence anisotropy vs. time that contain no peaks that are distinguishable from the noise of the anisotropy background into plots that show distinct fluorescence anisotropy peaks. The method was demonstrated using laser-induced fluorescence anisotropy data from individual Aβ (1–42) aggregates separated using capillary electrophoresis. Applying this data treatment method enabled the detection of anisotropy peaks for individual Aβ aggregate fluorescence peaks that were not observed prior to the data treatment method. The data treatment method is not specifically designed for Aβ aggregate analysis or capillary electrophoresis, and it should be applicable to other applications and other separation methods with FA detection.     

Solid-phase extraction of vitamins A and E from animal feeds: A substitute for liquid--liquid extraction

A substitution was developed for the laborious liquid-liquid extraction method according to European Economic Community legislation for isolation of Vitamins A and E from feeds. A rapid method for the isolation of the 2 vitamins by means of solid-phase extraction on OASIS columns gave reproducible results comparable to those of the European Union-recommended method. The vitamins in the feed were extracted with a minor modification of the official method (KOH in ethanol). After filtration, a portion was applied onto the OASIS column and then washed. The vitamins were eluted in ethyl acetate. The eluate evaporated under nitrogen, and the precipitate was dissolved in methanol before liquid chromatography analysis. Recovery for this method was 80% for Vitamin A and 110% for Vitamin E, as calculated as the result for National Institute of Standards and Technology (NIST) Infant Formula. Day-to-day reproducibility for the method was 21 and 11% of the average results for Vitamins A and E, respectively.     

Continuous ultrasound-assisted extraction of hexavalent chromium from soil with or without on-line preconcentration prior to photometric monitoring

A continuous ultrasound-assisted extractor was coupled to a photometric detector in order to obtain a fully automated approach for the determination of CrVI in soil. The use of a flow injection (FI) manifold as interface between the extractor and the photometric detector allowed the monitoring of CrVI after extraction in a continuous manner. The coloured complex formed between 1,5-diphenylcarbazide (DPC) and CrVI was used as recommended in EPA method 7196A because it is one of the most sensitive and selective reactions for CrVI determination. A preconcentration minicolumn packed with a strong anion-exchange resin was placed between the extractor and the detector, providing a more sensitive method. The linear dynamic ranges were 1-10 and 0.25-7.5 mg l-1 for the methods without (method A) and with preconcentration (method B), respectively. The limits of detection were 4.52 ng for method A and 1.23 ng for method B. Both methods were applied to a natural contaminated soil and the results obtained agreed well with those obtained by the reference EPA method 3060A. The influence of different amounts of CrIII in the samples was also studied and the results showed that the proposed methods did not disturb the original species distribution.     

An improved poly(A) motifs recognition method based on decision level fusion

Polyadenylation is the process of addition of poly(A) tail to mRNA 3′ ends. Identification of motifs controlling polyadenylation plays an essential role in improving genome annotation accuracy and better understanding of the mechanisms governing gene regulation. The bioinformatics methods used for poly(A) motifs recognition have demonstrated that information extracted from sequences surrounding the candidate motifs can differentiate true motifs from the false ones greatly. However, these methods depend on either domain features or string kernels. To date, methods combining information from different sources have not been found yet. Here, we proposed an improved poly(A) motifs recognition method by combing different sources based on decision level fusion. First of all, two novel prediction methods was proposed based on support vector machine (SVM): one method is achieved by using the domain-specific features and principle component analysis (PCA) method to eliminate the redundancy (PCA–SVM); the other method is based on Oligo string kernel (Oligo-SVM). Then we proposed a novel machine-learning method for poly(A) motif prediction by marrying four poly(A) motifs recognition methods, including two state-of-the-art methods (Random Forest (RF) and HMM-SVM), and two novel proposed methods (PCA–SVM and Oligo-SVM). A decision level information fusion method was employed to combine the decision values of different classifiers by applying the DS evidence theory. We evaluated our method on a comprehensive poly(A) dataset that consists of 14,740 samples on 12 variants of poly(A) motifs and 2750 samples containing none of these motifs. Our method has achieved accuracy up to 86.13%. Compared with the four classifiers, our evidence theory based method reduces the average error rate by about 30%, 27%, 26% and 16%, respectively. The experimental results suggest that the proposed method is more effective for poly(A) motif recognition.     

Direct quantitative determination of cyanamide by stable isotope dilution gas chromatography-mass spectrometry

Cyanamide is a multifunctional agrochemical used, for example, as a pesticide, herbicide, and fertilizer. Recent research has revealed that cyanamide is a natural product biosynthesized in a leguminous plant, hairy vetch (Vicia villosa). In the present study, gas chromatography-mass spectrometry (GC-MS) equipped with a capillary column for amines was used for direct quantitative determination of cyanamide. Quantitative signals for ((14)N(2))cyanamide, ((15)N(2))cyanamide (internal standard for stable isotope dilution method), and m-(trifluoromethyl)benzonitrile (internal standard for correcting errors in GC-MS analysis) were recorded as peak areas on mass chromatograms at m/z 42 (A(42)), 44 (A(44)), and 171 (A(IS)), respectively. Total cyanamide content, ((14)N(2))cyanamide plus ((15)N(2))cyanamide, was determined as a function of (A(42)+A(44))/A(IS). Contents of ((14)N(2))cyanamide and ((15)N(2))cyanamide were then calculated by multiplying the total cyanamide content by A(42)/(A(42)+A(44)) and A(44)/(A(42)+A(44)), respectively. The limit of detection for the total cyanamide content by the GC-MS analysis was around 1ng. The molar ratio of ((14)N(2))cyanamide to ((15)N(2))cyanamide in the injected sample was equal to the observed A(42)/A(44) value in the range from 0.1 to 5. It was, therefore, possible to use the stable isotope dilution method to quantify the natural cyanamide content in samples; i.e., the natural cyanamide content was derived by subtracting the A(42)/A(44) ratio of the internal standard from the A(42)/A(44) ratio of sample spiked with internal standard, and then multiplying the resulting difference by the amount of added ((15)N(2))cyanamide (SID-GC-MS method). This method successfully gave a reasonable value for the natural cyanamide content in hairy vetch, concurring with the value obtained by a conventional method in which cyanamide was derivatized to a photometrically active compound 4-cyanimido-1,2-naphthoquinone and analyzed with reversed-phase HPLC (CNQ-HPLC method). The determination range of cyanamide in the SID-GC-MS method was almost the same as that in the CNQ-HPLC method; however, the SID-GC-MS method was much simpler than the CNQ-HPLC method.     

吖啶橙指示荧光分析法测定双酚A

基于在酸性介质中,双酚A对羟自由基与吖啶橙的氧化还原反应的阻抑作用,建立了测定双酚A的荧光分析新方法.该方法简单,快速,线性范围为1.0～100 ng/mL,检出限为0.21 ng/mL.将其用于塑料制品中双酚A的测定,结果满意.     

用溴酸钾-丁基罗丹明B体系动力学荧光法测定双酚A

在盐酸介质中,双酚A对溴酸钾氧化丁基罗丹明B荧光猝灭具有抑制作用,据此建立了动力学荧光法测定痕量双酚A的新方法。方法的线性范围是0.08～0.88mg/L。检出限为0.005 mg/L,回收率在95%～103%之间。该方法已用于婴幼儿奶瓶、假牙和地表水中双酚A含量的测定,结果满意。     

烟草中烟碱的水相萃取和液相色谱分析

本文系统地研究了烟草中烟碱的水相萃取,建立了测定烟碱的萃取-色谱法。此法不仅简单、准确,而且克服了传统蒸馏法测定结果偏低的弊端。     

金属和试剂分别过量时测定不同配合物组成的新方法

金属和试剂分别过量时测定不同配合物组成的新方法何锡文,唐志新,张贵珠,杨万龙,于贵英,史慧明（南开大学化学系,天津,３０００７１）关键词配合物组成,穷举法,光度分析本文用穷举法推导了一种新的数学模型,该法不需要假定配合比,就能测定当试剂和金属分别过量...     

High-performance liquid chromatographic analysis of norepinephrine and alpha-methylnorepinephrine in microdissected noradrenergic cell groups of the rabbit brain

A high-performance liquid chromatographic method with electrochemical detection has been developed to measure norepinephrine (NE) and alpha-methylnorepinephrine (alpha-MeNE) in microdissected noradrenergic cell groups of the rabbit brain stem. The method is shown to be specific, accurate and precise and has a sensitivity of 0.5 pmol per sample. The method has been applied to the measurement of NE and alpha-MeNE levels in the A1, A2, A5, A6 and A7 noradrenergic cell groups after administration of the antihypertensive drug alpha-methyldopa (alpha-MD), so that the sites of action of alpha-MD within the central nervous system may be localised.     

火焰原子吸收法测定油画颜料中铅含量

采用干灰化法、湿氧化A法和B法分别对油画颜料进行消解后用原子吸收火焰法测定其中的铅含量.通过分析比较3种消解方法测定的结果,发现采用湿氧化法优于干灰化法,湿氧化A法优于B法.采用湿氧化A法对油画颜料进行加标处理后,加标回收率在90%-105%范围,表明采用该方法测定油画颜料中的铅含量是可信的.     

Birefringence of highly oriented fibers

A spectrophotometric method was developed for measuring the birefringence of highly oriented synthetic fibers. This method surmounts the low birefringence limit of the standard quartz compensator method and the difficulties in interpretation of the photographic fringe method. A highly oriented aramid fiber gave birefringence values of 0.60–0.75 by this method, compared with 0.25 for polyester and 0.06 for nylon by other conventional methods. The operating principles and excellent results of this new method provide a basis for the extension of routine birefringence characterization to highly oriented fibers.     

H‐Point Standard Addition Method Applied to Voltammetry of Microparticles. Quantitation of Dyes in Pictorial Samples

A solid‐state electrochemical application of the H‐point standard addition method (HPSAM) for quantifying two electroactive compounds, A, B, that produce strongly overlapped voltammetric peaks is described. It is based on peak current measurement in square‐wave voltammograms recorded for solid samples containing a reference compound R, upon additions of a A‐ (or B‐) containing standard compound. The method allows to the determination of the mass fraction of A and B by applying the H‐point standard addition method to solid state voltammetry. The quotients between the currents measured at two selected potentials and the peak current of R vary linearly with the mass ratio of the added standard and the reference compound, thus providing an electrochemical method for determining the content of A and B in the sample avoiding matrix effects. The method is applied to the simultaneous determination of alizarin and purpurin in madder pigments and pictorial specimens using morin as a reference material.     

Long-chain branching in low-density polyethylene

A method is given for the analysis of long-chain branching in polymers by using combined GPC and intrinsic viscosity measurements. A computer program was written to evaluate branching indices by a tabular, iterative method. The method was applied to the evaluation of long-chain branching in low-density polyethylene.     

非线性主成分回归分光光度法同时测定复方制剂中两组分的含量

构造多组分体系的非线性模型,并用主成分回归法来解析,建立了同时测定两组分的非线性主成分回归分光光度法,方法用于复方苯甲酸制剂中苯甲酸和水杨酸含量的测定,结果优于线性主成分回归分光光度法。     

Solid-phase extraction applied to the determination of ochratoxin A in wines by reversed-phase high-performance liquid chromatography

A reversed-phase high-performance liquid chromatographic method is described for the analysis of Ochratoxin A at low microg l(-1) levels in samples of artificially contaminated wines. The method involves solid-phase extraction of samples using octadecylsilane cartridges and an additional preconcentration step prior to chromatography with isocratic elution and fluorimetric detection. The method was evaluated for accuracy and precision with relative standard deviations lower than 10%. Recoveries of ochratoxin A added to commercial wines over the range 0.1-3.0 microg l(-1) were higher than 80% in the assays. The performance of the octadecylsilane cartridge method tested compared very favourably with results of other published studies of ochratoxin A which use immunoaffinity columns or solvent extraction techniques.     

Rapid and simple method for the determination of alpha 1-acid glycoprotein in serum by column liquid chromatography.

A rapid and simple method for the determination of alpha 1-acid glycoprotein (AAG) in serum was developed by using an anion-exchange column for clean-up of serum and a hydroxyapatite column for high-performance liquid chromatography (HPLC). A good correlation was observed between this HPLC method and the conventional radial immunodiffusion method. The method may also be used to determine the AAG concentration in the serum of experimental animals.