Application of HPLC to measure vanadium in environmental,biological and clinical matrices

Vanadate and vanadium compounds exist in many environmental, biological and clinical matrices, and despite the need only limited progress has been made on the analysis of vanadium compounds. The vanadium coordination chemistry of different oxidation states is known, and the result of the characterization and speciation analysis depends on the subsequent chemistry and the methods of analysis. Many studies have used a range of methods for the characterization and determination of metal ions in a variety of materials. One successful technique is high performance liquid chromatography (HPLC) that has been used mainly for measuring total vanadium level and metal speciation. Some cases have been reported where complexes of different oxidation states of vanadium have been separated by HPLC. Specifically reversed phase (RP) HPLC has frequently been used for the measurement of vanadium. Other HPLC methods such as normal phase, anion-exchange, cation-exchange, size exclusion and other RP-HPLC modes such as, ion-pair and micellar have been used to separate selected vanadium compounds. We will present a review that summarizes and critically analyzes the reported methods for analysis of vanadium salts and vanadium compounds in different sample matrices. We will compare various HPLC methods and modes including sample preparation, chelating reagents, mobile phase and detection methods. The comparison will allow us to identify the best analytical HPLC method and mode for measuring vanadium levels and what information such methods provide with regard to speciation and quantitation of the vanadium compounds.     

Conversion of phosphogypsum to potassium sulfate

Summary Solubility of calcium sulfate in concentrated aqueous chloride solutions is of particular significance in chloride hydrometallurgy and various crystallization processes, such as the production of potassium sulfate from phosphogypsum and potassium chloride. This paper examines an example of the second type of application in which gypsum and potassium chloride are reacted to form K₂SO₄. The solubility of phosphogypsum in aqueous solutions of KCl, HCl, and mixtures of both has first been measured at various temperatures and concentrations. The parameters investigated are HCl concentration up to 6M, KCl concentration up to 180 g L^-1 and temperature from 25 to 80°C. In addition, the influence of co-existing chloride salts, such as (HCl+KCl), on the solubility of calcium sulfate is estimated from 25 to 80°C. The solubility increases obviously with the temperature increment as it does initially with acid concentration, reaching a maximum of about 3M HCl, 130 g L^-1 KCl and then drops. At the same time, the solubility of CaSO₄·2H₂O decreases with increasing KCl concentration.     

Development and Validation of Kinetic Spectrophotometric Method for the Determination of Losartan Potassium in Pure and Commercial Tablets

A validated kinetic spectrophotometric method has been developed for the determination of losartan potassium in pure and dosage forms. The method is based on oxidation of the losartan potassium with alkaline potassium permanganate at room temperature (25 ± 1 °C). The reaction is followed spectrophotometrically by measuring the increase in absorbance with time at 603 nm, and the initial rate, fixed time (at 12.0 min) and equilibrium time (at 90.0 min) methods are adopted for constructing the calibration graphs. All the calibration graphs are linear in the concentration range of 7.5–60.0 μg mL^?1 and the calibration data resulted in the linear regression equations of n? = ?6.422 × 10^?7 + 1.173 × 10^?5 C, A =3.30 × 10^?4 + 5.28 × 10^?3 C and A = ?2.09 × 10^?2 + 1.05 × 10^?1 C for initial‐rate, fixed time and equilibrium time methods, respectively. The limits of detection for initial rate, fixed time and equilibrium time methods are 0.71, 0.21 and 0.19 μg mL^?1, respectively. The activation parameters such as E_a, ΔH^?, ΔS^?, and ΔG^? are also determined for the reaction and found to be 87.34 KJ mol^?1, 84.86 KJ mol^?1, 50.96 JK^?1 mol^?1 and ?15.10 KJ mol^?1, respectively. The variables are optimized and the proposed methods are validated as per ICH guidelines. The method has been applied successfully to the estimation of losartan potassium in commercial tablets. The performance of the proposed methods was judged by calculating paired t‐ and F‐ values. The analytical results of the proposed methods when compared with those of the reference method show no significant difference in accuracy and precision and have acceptable bias.     

流动注射化学发光法测定柠檬酸

在H2 SO4介质中 ,高锰酸钾可以直接氧化柠檬酸产生化学发光 ,由此我们建立了流动注射化学发光测定柠檬酸的新方法。该方法测定柠檬酸的线性范围为 1× 1 0 -5～ 1× 1 0 -3g/mL ,方法的检出限为 3× 1 0 -6g/mL ,相对标准偏差r=2 % ( 1 .0× 1 0 -4g/mL ,n =1 1 ) ,该法已用于饮料中柠檬酸的含量测定     

钾盐在卷烟工业中的应用

介绍了国内外无机钾盐和有机钾盐在卷烟中的应用情况,对其研究现状作了简要的评述,并对将来的研究方向进行了展望.     

化学发光法快速测定亚甲蓝

在H2SO4介质中，KMnO4氧化亚甲蓝产生化学发光，甲醛显著增强该体系的发光强度，据此建立了一种简单、快速测定亚甲蓝的流动注射化学发光新方法．在优化的实验条件下，该法测定亚甲蓝的线性范围为0．08～8．00μg／mL，对2．00μg／mL，亚甲蓝进行了11次平行测定，其相对标准偏差为3．22％．将本法用于血样、尿样及针剂中亚甲蓝的测定，结果令人满意。     

山梨酸钾/柠檬酸对番茄汁保藏的影响

探讨了山梨酸钾、柠檬酸分别与冷藏相结合的方法对番茄汁保藏的影响。试验结果表明:在8周的贮藏过程中,添加0.09%山梨酸钾的番茄汁,其可溶性固性物含量基本稳定,风味色泽变化不大,而添加0.03%和0.06%山梨酸钾的样品可溶性固形物下降15%。添加柠檬酸的样品与对照一样,可溶性固形物下降较大,风味色泽下降更多。所有样品维生素C含量、菌落总数均有较大下降,添加山梨酸钾的样品下降更大,说明山梨酸钾影响维生素C的保存。冷藏番茄汁时,添加0.09%的山梨酸钾更为有效。柠檬酸对番茄汁的保藏作用不大。     

叶用银杏林配方施肥效应初报

文章对银杏采叶林氮、磷、钾不同配比的施肥效果进行了研究。试验结果表明N、P、K不同配比施肥后，对银杏的叶片面积、单叶质量和单株产叶量有明显的增长效果，增长幅度分别为：9．2％-22．5％、14．3％-29．5％和19．0％-55．1％。尤以N：P2P5：K20为6：2：2的配比最为显著，增长幅度分别为22．5％、29．5％和55．1％。     

对"过氧化氢碘化钾催化分解"催化概念的质疑

在过氧化氢中加入碘化钾溶液，过氧化氢的分解速率显著加快．国内外文献普遍认为这是碘化钾在起催化剂作用．我们发现反应过程中溶液颜色变黄．进一步的实验表明，溶液中碘离子浓度降低、溶液的电导率增大、pH值升高，而且溶液中生成了单质碘．根据对上述实验研究结果，我们对碘化钾作为过氧化氢分解反应的催化剂的概念提出了质疑。并证实发生了过氧化氢氧化碘化钾的化学反应．     

铁氰化钾化学发光体系测定盐酸肾上腺素

基于铁氰化钾可以在碱性条件下直接氧化盐酸肾上腺素产生化学发光这一现象,并结合流动注射技术建立了一种直接测定盐酸肾上腺素的流动注射化学发光新方法.该方法的线性范围在5 0×10-8～5 0×10-6g/mL,检出限为2 8×10-9g/mL(3σ).对5 0×10-7g/mL的盐酸肾上腺素连续11次测定的相对标准偏差为3 2%.该法已成功测定了注射液中的盐酸肾上腺素含量,结果令人满意.