酸性络蓝K双波长信号系数光度法测定钙镁

基于在氢氧化钠溶液中,钙、镁均与酸性络蓝K(ACBK)形成暗红色配合物,提出了测定钙和镁的双波长信号系数光度法.该法不仅消除了钙、镁之间的吸收干扰,且消除了一定量的共存离子的干扰.利用褪色法与生色法的吸光度之和作为信号吸光度,使方法的灵敏度大为提高.测定钙、镁总量时,分别用钙、镁吸收曲线正峰与负峰上的等吸收波长470.5 nm(λPa)及559.5 nm(λNa)处测定吸光度APa和ANa,求得总量的信号系数fs为2.439.于λPa470.5 nm处测得任一浓度钙、镁试液的吸光度APa′,其信号吸光度As=fsAλPa′.测定镁时,以试剂ACBK褪色对钙配合物生色的完全相消干扰的波长539 nm(Pa)作为测定波长,负峰波长583 nm为Na.按相同方法测得镁的信号系数fs为4.148.     

高锰溶液中钙、镁含量的测定

在化工、冶金行业中,很多试验研究都涉及到溶液的成分分析,其中钙、镁的常规分析非常普遍.若遇到锰盐的溶液中常量钙、镁的测定,使用常规的分析方法将会遇到一些困难,因为溶液中大量锰离子的存在会对钙、镁测定结果的准确性产生较大的影响.     

计算机-原子吸收光谱法测定钙、镁、硫酸根等的含量

前言在硫酸盐等的存在下,对钙、镁的测定干扰严重,过去多用化学分离或改变光谱条件等方法进行测定。本文提出不经化学分离,利用计算机-原子吸收光谱方法,建立了一定的数学模型,直接测定并计算出钙、镁浓度及干扰组分硫酸根的浓度。用计算机处理方法及其数学模型可适用于类似情况的其他元素的测定。实验 1.原子吸收光谱测定条件:仪器为日本岛津AA—610S型。空气-乙炔火焰。单缝燃烧器,具体条件见表1。 2.实验结果:在钙、镁、钠、硫酸根等的共存试样中,分别做出纯钙、镁的工作曲线。在此基础上     

希土产品微量镁和钙的比色测定

希土产品中镁和钙的测定,一般选用氨水分离法,由于空白高,微量镁和钙有可能吸附,测定结果的准确度较差。本文用阳离子交换树脂使希土同镁和钙分离,并分别比色测定镁和钙。方法适用于0.0001—0.010％镁和0.0002—0.020％钙的测定(以1克样计算)。 (一) 试剂和仪器     

高钒试样中钙美的快速连续测定

高钒试样中钙的测定是在一定酸度条件下,在氯化铵存在下用草酸铵沉淀钙而与钒分离,然后用硫酸溶解,再用高锰酸钾标准溶液滴定[1]或将草酸钙灼烧为氧化钙后用EDTA络合滴定[2].这些方法分析流程长,操作复杂,并且对高含量镁的测定均没有详细报道.本文提出了一种简便、快速测定高钒试样中高含量钙和镁的方法.     

铝土矿中低含量钙、镁的连续比色测定——甲基百里酚蓝比色法

甲基百里酚蓝(MTB)作为镁的显色剂测定微量镁已有报导,但未见其应用于钙的测定。而MTB与钙也有良好的显色性能,本文提出在MTB与钙镁同时显色后,加入EGTA,利用其对钙镁络合物稳定常数的差别,仅使钙褪色,藉以连续比色测定试样中的钙和镁。方法特别适用于铝土矿等钙镁含量大致相当的试样中低含量钙镁的测定。一、主要试剂MTB(0.15%) 0.15克MTB和1克盐     

电感耦合等离子体原子发射光谱法测定中药材中钙、镁和磷

应用电感耦合等离子体原子发射光谱法同时测定了3种中药材(淫羊藿、杜仲及肉苁蓉)中生物元素钙、镁及磷的含量.用干灰化法处理药材试样,残渣用硝酸溶解并以水定容后备作AES测定.选择波长为 317.933,280.271 及 214.914 nm 3条分析谱线分别测定钙、镁及磷3元素的含量.3元素的检出限依次为 10.0,1.6 及 140.0 mg·L-1.应用所提出的方法测定了上述3种中药材中的钙、镁和磷的含量,算得 3 元素的相对标准偏差(n=7)均小于3%.     

钙镁同时测定的新显色剂偶氮氯膦-mB

本文记述了用新显色剂偶氮氯膦-mB分光光度法同时测定钙、镁。在pH10.3左右的氨性溶液中,显色剂与钙、镁同时形成很稳定的2:1配合物,表观摩尔吸光系数分别为ε_(635)~(Ca)=1.5×10~4。ε_(575)~(Mg)=1.2×10~4。在同一试液中直接测定钙量和镁量。对于钙含量高的试样:先测定钙量,再用EGTA-Mo,掩蔽钙后测定镁量。本方法操作简便、快速,易于掌握,测定范围宽,结果稳定可靠,优于迄今报道的其它同时光度法测定钙、镁的显色剂。     

双波长吸光光度法同时测定血清中钙和镁

血清中钙和镁与人的健康密切相关,由于性质接近,又往往共存,给分析带来一定的困难.钙和镁同时测定报道不多,常用原子吸收光度法,虽灵敏可靠,但仪器昂贵.本法可同时测定血清中钙和镁,无需分离和加掩蔽剂,方法简便、快速、结果可靠.甲基百里香酚蓝(MTB)是一种优良的金属络合染料,在碱性条件下只与钙、镁离子呈色.本文利用等吸收双波长消去法,在选定的两波长处,干扰组分具有相等的吸光度,钙、镁混合物吸光度的差值△A只与待测组分的浓度成正比,由此可计算待测组分的浓度.1试验部分1.1主要仪器与试剂     

稀土镁合金中镁的快速分析

稀土镁合金中镁的测定,目前大多采用差减法,即测定钙、镁合量后,然后减去钙的含量,得到镁量。速度既慢,而且当测定钙造成误差时,将直接影响到镁的测定结果。本法避免了以上缺点,钙首先用EGTA络     

Automatic registration for images of two-dimensional protein gels.

Two-dimensional polyacrylamide gel electrophoresis 1 (2-D PAGE 1) is currently the method of choice for separating complex mixtures of cellular proteins. Despite its usefulness, 2-D PAGE is not being applied to its full potential because of difficulties with both the method and analysis of the results. One of the key problems is the difficulty and slowness of image analysis, especially registration (image alignment), which is laborious and the results unsatisfactory. We have developed a novel system for analysis of 2-D PAGE images, called Z3, that performs the analysis faster and more precisely. The Z3 system employs novel approaches to image registration, image display, computation of differential expression, and the design and analysis of 2-D gel experiments. This paper describes in detail the registration algorithm, and briefly discusses the merits of complementary pseudocolor display. The registration algorithm is novel in that for the first time raw-image-based registration technology is applied to 2-D gel analysis.     

Simple fluorimetric liquid chromatographic method for the analysis of undecylenic acid and zinc undecylenate in pharmaceutical preparations

A simple and selective liquid chromatographic method is described for the analysis of undecylenic acid (UA) and zinc undecylenate (ZnUA) in pharmaceutical preparations. The method is based on the derivatization of the analytes extracted from various samples with 2-(2-naphthoxy)ethyl 2-(piperidino)ethanesulfonate. The resulting derivative was analyzed by liquid chromatography with fluorimetric detection. The quantitation of the method is in the range of 3.0-50.0 microM UA with a detection limit of about 0.3 microM (S/N = 3 with 10 microl injection). We found that acetonitrile is a selective solvent for differentially dissolving UA from coexisted ZnUA in compound formulation. This results in the specific analysis of UA in the presence of ZnUA and simply analyzing the coexisted ZnUA by the value of total UA (UA+ZnUA) minus that of UA. Application of the method to the analysis of undecylenic acid and zinc undecylenate in ointment, powder and solution preparations proved feasible.     

X射线荧光光谱法测定萤石中的氟,钙及二氧化硅

提出艇偏硼酸锂和四硼酸锂混合熔剂熔融制样，以Ｘ－射线荧光光谱法定量测定萤石中ＣａＦ２、总钙和二氧化硅。经实际试样和标准试样检测，本法可用实际试样分析，在ＣａＦ２含量为７７－９８％时，其最大误差为０．６０％。     

Microchip electrophoresis for specific gene detection of the pathogenic bacteria V. cholerae by circle-to-circle amplification.

We have developed a new method for a fast and precise analysis of circle-to-circle amplification (C2CA) product for specific gene detection by microchip electrophoresis. In this method, we have added a new enzymatic step to the C2CA reaction, which could be carried out isothermally at 37 degrees C. Compared to the original single-stranded DNA, the double-stranded DNA that is produced by this enzymatic reaction is more reliable for analysis by microchip electrophoresis. C2CA product was detected within 55 s with high reproducibility by this method which was successfully applied to the detection of 10-ng genomic DNA of the pathogenic bacteria Vibrio. cholerae within 110 s. Purification was found to be an indispensable step for the analysis of the C2CA product of genomic DNA samples.     

Effective protein extraction protocol for proteomics studies of Jerusalem artichoke leaves

Protein extraction is a crucial step for proteomics studies. To establish an effective protein extraction protocol suitable for two‐dimensional electrophoresis (2DE) analysis in Jerusalem artichoke (Helianthus tuberosus L.), three different protein extraction methods—trichloroacetic acid/acetone, Mg/NP‐40, and phenol/ammonium acetate—were evaluated using Jerusalem artichoke leaves as source materials. Of the three methods, trichloroacetic acid/acetone yielded the best protein separation pattern and highest number of protein spots in 2DE analysis. Proteins highly abundant in leaves, such as Rubisco, are typically problematic during leaf 2DE analysis, however, and this disadvantage was evident using trichloroacetic acid/acetone. To reduce the influence of abundant proteins on the detection of low‐abundance proteins, we optimized the trichloroacetic acid/acetone method by incorporating a PEG fractionation approach. After optimization, 363 additional (36.2%) protein spots were detected on the 2DE gel. Our results suggest that trichloroacetic acid/acetone method is a better protein extraction technique than Mg/NP‐40 and phenol/ammonium acetate in Jerusalem artichoke leaf 2DE analysis, and that trichloroacetic acid/acetone method combined with PEG fractionation procedure is the most effective approach for leaf 2DE analysis of Jerusalem artichoke.     

Development and validation of a capillary high-performance liquid chromatography/electrospray tandem mass spectrometric method for the quantification of bisphenol A in air samples

Bisphenol A (BPA) is a toxic industrial chemical that affects the endocrine system even at low concentrations. A new method, based on capillary high-performance liquid chromatography/electrospray ionization tandem mass spectrometry (HPLC/ESI-MS/MS) analysis, has been developed to determine BPA in atmospheric samples. The method involves collection of air samples (typically 2 m(3)) on glass fiber filters, with ultrasonic extraction and sample concentration under vacuum before analysis. HPLC analysis was performed isocratically at a flow rate of 10 microL min(-1) using a capillary reversed-phase column and MS/MS analysis in negative ion multiple reaction monitoring (MRM) mode, using BPA-d(16) as internal standard. The present method provides linear response in the range 0.007-3.5 microg/filter (R(2) > 0.999) and is characterized by high accuracy (mean bias 2%) and good reproducibility (mean RSD 5%). High sensitivity (LOD = 2 ng/m(3) based on 2 m(3) of air collected), specificity, and speed of the analysis make the present method suitable for routine determination of BPA in the atmosphere, both for ambient and personnel monitoring.     

Peak clustering in two-dimensional gas chromatography with mass spectrometric detection based on theoretical calculation of two-dimensional peak shapes: the 2DAid approach

A method is presented to facilitate the non-target analysis of data obtained in temperature-programmed comprehensive two-dimensional (2D) gas chromatography coupled to time-of-flight mass spectrometry (GC×GC-ToF-MS). One main difficulty of GC×GC data analysis is that each peak is usually modulated several times and therefore appears as a series of peaks (or peaklets) in the one-dimensionally recorded data. The proposed method, 2DAid, uses basic chromatographic laws to calculate the theoretical shape of a 2D peak (a cluster of peaklets originating from the same analyte) in order to define the area in which the peaklets of each individual compound can be expected to show up. Based on analyte-identity information obtained by means of mass spectral library searching, the individual peaklets are then combined into a single 2D peak. The method is applied, amongst others, to a complex mixture containing 362 analytes. It is demonstrated that the 2D peak shapes can be accurately predicted and that clustering and further processing can reduce the final peak list to a manageable size.     

水溶性聚胺PEI与铜离子螯合物结构的测定及其分析应用

使用分光光度法与电导滴定法研究了聚乙烯亚胺（PEI）与Cu^2＋的配合过程,测定了二者所形成的螯合物结构。Cu^2＋与水溶性聚胺PEI可以定量地形成四配位螯合物,而且配合过程速度很快,螯合物稳定;在用PEI水溶液滴定Cu^2＋过程中,体系的电导率快速下降,在滴定终点电导率发生了清晰的转变。建立了测定Cu^2＋的一种新方法-PEI螯合作用电导滴定法,考察了各种因素对分析方法的影响,优化了分析条件。     

Application of a New Dehydroascorbic Acid Reducing Agent in the Analysis of Vitamin C Content in Food

The analysis of total vitamin C content in food is most frequently performed by reducing dehydroascorbic acid to ascorbic acid, which is then assayed with the technique of high-performance liquid chromatography combined with spectrophotometric detection. Tris(2-carboxyethyl)phosphine is currently the only agent in use that efficiently reduces dehydroascorbic acid at pH < 2. Therefore, there is a continued need to search for new reducing agents that will display a high reactivity and stability in acidic solutions. The objective of the study was to verify the applicability of unithiol and tris(hydroxypropyl)phosphine for a reducing dehydroascorbic acid in an extraction medium with pH < 2. The conducted validation of the newly developed method of determining the total content of vitamin C using tris(hydroxypropyl)phosphine indicates its applicability for food analysis. The method allows obtaining equivalent results compared to the method based on the use of tris(2-carboxyethyl)phosphine. The low efficiency of dehydroascorbic acid reduction with the use of unithiol does not allow its application as a new reducing agent in vitamin C analysis.