Simultaneous Determination of Norfloxacin and Tinidazole in Tablets by Reverse Phase High Performance Liquid Chromatography (RP - HPLC).

Abstract

A new simple, precise, rapid and selective HPLC-RP method has been developed for the simultaneous determination of Norfloxacin and Tinidazole in formulations, using 0.2 % Triethylamine (TEA) in water : Acetonitrile (80:20,v/v) and pH adjusted to 2.6 to 2.8 with Phosphoric acid, as a mobile phase, and C₁₈ SHODEX column (5 micron, 25 cm × 3.9 mm, ID) as stationary phase. Detection was carried out using a UV detector at 311 nm Linearity range and percentage recoveries for Norfloxacin and Tinidazole were 20 - 200 μg/mL and 30 - 300 μg/mL, 999.91 % and 99.94 % respectively.     

Capillary liquid chromatography with UV detection using N,N-diethyl dithiocarbamate for determining platinum-based antitumor drugs in plasma

A capillary liquid chromatography with UV detection (CLC-UV) system has been developed for determining platinum-based antitumor drugs (e.g., cisplatin, carboplatin, and nedaplatin) in plasma based on the pre-column derivatization of platinum with N,N-diethyl dithiocarbamate (DDTC). The chelated platinum separation was carried out on a capillary column (Inertsil ODS-3, 150 mm × 0.3 mm i.d., 3 μm) using an acetonitrile-water mixture (8:2, v/v) as a mobile phase that flowed at 5.0 μL/min. Detection was carried out by absorbance at 254 nm. Chromatographic peak height was found to be linearly related to the spiked concentration of nedaplatin in the blank control plasma from 5.0 ng/mL to 15 μg/mL (r(2)>0.998). The repeatability (n=5) of the chromatographic peak height for 2.5 μg/mL nedaplatin was 2.6% relative standard deviation (R.S.D.). The CLC-UV system, which required only 20 μL of plasma sample, was applied to the determination of total and free form platinum-based antitumor drugs in plasma after injection into rats. The recovery rates (n=5) of total and free form nedaplatin in plasma were 98% and 99%, respectively, and these repeatability were 2.4% R.S.D. and 3.1% R.S.D., respectively. In addition, the recovery rates (n=5) of total and free form carboplatin in plasma were 99% and 99%, respectively, and these repeatability were 2.9% R.S.D. and 0.24% R.S.D., respectively. The concentration-time profiles of total and free form nedaplatin in rat plasma were monitored to determine the pharmacokinetic parameters.     

Liquid Chromatographic Analysis of Cephalexin in Human Plasma by Fluorescence Detection of the 9-Fluorenylmethyl Chloroformate Derivative

Abstract

A simple and sensitive precolumn derivatization method for the determination of cephalexin in human plasma has been developed. Cephalexin was derived with 9-fluorenylmethyl chloroformate (FMOC-Cl) in borate buffer (5 mM, pH 8.5) for 15 min at 25°C. Optimal conditions for the derivatization were described. The derivative was chromatographed on an XDB-C₁₈ column with water–acetonitrile (10:90, v/v) as mobile phase at a flow rate of 1.0 mL/min. The fluorescence excitation and emission wavelengths were 268 nm and 314 nm, respectively. The standard curve in spiked plasma was linear over the range of 0.0234–58.5 µg/mL; the detection limit (signal-to-noise ratio = 3; injection volume, 10 µL) was about 0.014 µg/mL. The performance of analysis was studied, and the validated method showed excellent performance in terms of selectivity, sensitivity, precision, and accuracy.     

Quantitative Determination by Using HPLC and GLC Methods for Cocaine HCl in Synthetic Binary Mixtures with Procaine HCl,Lidocaine HCl and Caffeine

ABSTRACT

Cocaine HCl is a substance which creates psychological and physical dependence. Usually it is available on the market being diluted by other substances, like local anesthetics, analeptics and CNS stimulating agents and inert substance.

In this study, HPLC and GLC methods were applied for qualitative and quantitative determinations of synthetic binary mixtures. In the HPLC determination, μ Bondopack C₁₈ 10 μm. column system, a mobile phase consisting of methanol-water-phosphoric acid-1% hexylamine (75:175:250:3,5) and U.V. detection by photodiodearray (196–600 nm) were used.

The linear concentration areas were found in a range of 2.5–25 μg/mL. The R.S.D percentages for cocaine HCl, procaine HCl, lidocaine HCl and caffeine were found as 0.922, 0.568, 1.18 and 1.04, respectively.

In the GLC determination, two different column systems, a 2% OV-17-Gas Chrom W-HP 100–200 mesh filled column and a 0.25 SE-52 fused silica capillary column, were used. Nitrogen was used in a filled column and helium was used in a capillary column. Mobile phase flow rates were set as 30 mL/min and a flame ionization detector was used with both column systems.

The linear concentration intervals were found in a range of 2–25 μL/mL in both methods. The R.S.D. for cocaine HCl, procaine HCl, lidocaine HCl, and caffeine were found to be 0.907, 0.948, 0.770, 0.901 in the filled column. For cocaine HCl, procaine HCl and caffeine R.S.D.'s of 0.774, 0.809, 0.814 were found, when a capillary column was used. In quantitative determinations, antipyrine was chosen as internal standard in the HPLC and GLC methods.     

Determination of Amphotericin-B in Human Plasma by Reversed-Phase High Performance Liquid Chromatography Using a Short Octyl Column

Abstract

Amphotericin-B is a polyene antifungal antibiotic used for the treatment of severe systemic fungal infections. For effective treatment of urinary fungaria and the prevention of significant adverse-effects, monitoring the concentration of Amphotericin-B in biological samples of humans (ingesting the drug) is required. In this experiment, Amphotericin-B was isolated from plasma endogenous substances by adding 200 μL of acetonitrile in 800 μL of plasma. This mixture was vortex mixed, 20 mg of zinc sulfate and 10 mg of monobasic potassium phosphate was added to the mixture. This mixture was again vortex mixed and followed by centrifugation. The supernatant was filtered through a 0.45 μm membrane and a 100 μL aliquot of this solution was injected onto the chromatographic system. A short column of 60 mm × 4.6 mm packed with 3 μm octyl particles was used with an isocratic elution of 50/50, acetonitrile/0.01M KH₂PO₄ (v/v). The pH of the mobile phase mixture was adjusted to 3.5 with H₃PO₄. The intact drug molecule (parent drug) was monitored by a W-visible detector at 410 nm and 0.10-0.005 A.U.F.S. The limits of detection of the method were 0.03 μg/mL for 100 μl injection volume at signal-to-noise ratio of 3.     

An HPLC‐UV method for determining plasma dimethylacetamide concentrations in patients receiving intravenous busulfan

Dimethylacetamide (DMA) is a solvent used in the preparation of intravenous busulfan, an alkylating agent used in blood or marrow transplantation. DMA may contribute to hepatic toxicity, so it is important to monitor its clearance. The aim of this study was to develop an HPLC‐UV assay for measurement of DMA in human plasma. After precipitation of plasma proteins with acetonitrile followed by dilution (1:4) with water, the extract was injected onto the HPLC and detected at 195 nm. Separation was performed using a Cogent‐HPS 5 μm C₁₈ column (250 × 4.6 mm) preceded by a Brownlee 7 μm RP₁₈, pre‐column (1.5 cm × 3.2 mm). The mobile phase was 25 mm sodium phosphate buffer (pH 3), containing 2.5% (v /v) acetonitrile and 0.0005% (v /v) sodium‐octyl‐sulfonate. Using a flow rate of 1 mL/min, the retention times of DMA and the internal standard (IS), 2‐chloroacetamide, were 9.5 and 3.5 min, respectively. Peak area ratio (DMA:IS) was a linear function of concentration from 1 to 1000 μg/mL. There was excellent intraday precision (<5% for 5–700 μg/mL DMA), accuracy (<3% deviation from the true concentration) and recovery (74–98%). The limits of detection and quantification were 1 and 5 μg/mL, respectively. In eight children who received intravenous busulfan, DMA concentrations ranged from 110 to 438 μg/mL.     

Comparison of C18 silica and multi‐walled carbon nanotubes as the adsorbents for the solid‐phase extraction of Chlorpyrifos and Phosalone in water samples using HPLC

A comparison between C₁₈ silica and multi‐walled carbon nanotubes (MWCNTs) in the extraction of Chlorpyrifos and Phosalone in environmental water samples was carried out using HPLC. Parameters affecting the extraction were type and volume of elution solvent, pH and flow rate of sample through the adsorbent. The optimum conditions obtained by C₁₈ cartridge for adsorption of these pesticides were 4 mL dichloromethane as elution solvent, sample pH of 5, flow rate of 1 mL/min, and those for MWCNT cartridge were 3 mL dichloromethane, pH of 5 and flow rate of 10 mL/min, respectively. Optimized mobile phase for separation and determination of these compounds by HPLC was methanol/water (80:20 v/v) with pH=5 (adjusted with phosphate buffer). Under optimal chromatographic and SPE conditions, LOD, linear range and precision (RSD n=8) were 3.03×10^?3, 0.01–5.00 μg/mL and 2.7% for Chlorpyrifos and 4.03×10^?4, 0.01–5.00 μg/mL and 2.3% for Phosalone, in C₁₈ cartridge, respectively. These values for MWCNT were 4.02×10^?6, 0.001–0.500 μg/mL and 1.8% for Chlorpyrifos and 1.02×10^?6, 0.001–0.500 μg/mL and 1.5% for Phosalone, respectively.     

Determination of the epimerization rate constant of amygdalin by microemulsion electrokinetic chromatography

A new method for separation and determination of amygdalin and its epimer (neoamygdalin) in the epimerization of amygdalin by MEEKC is proposed. For the chiral separation of amygdalin and neoamygdalin, a running buffer composed of 80 mM sodium cholate, 5.0% v/v butan‐1‐ol, 0.5% v/v heptane and 94.5% v/v 30 mM Na₂B₄O₇ buffer (pH 9.00) is proposed. Under optimum conditions, the basic separation of amygdalin and neoamygdalin can be achieved within 7 min. The calibration curve for amygdalin showed excellent linearity in the concentration range of 20–1000 μg/mL with a detection limit of 5.0 μg/mL (S/N=3). The epimerization rate constant of amygdalin in basic microemulsion was first determined by monitoring the concentration changes of amygdalin, and the epimerization rate constant of amygdalin was found to be 2×10^?3 min^?1 at 25°C under the above optimum microemulsion conditions.     

High‐performance liquid chromatographic method for identification and quantification of three potent liver protective coumarinolignoids—cleomiscosin A,cleomiscosin B and cleomiscosin C—in extracts of Cleome viscosa

A simple, rapid, accurate and reproducible reverse‐phase HPLC method has been developed for simultaneous identification and quantification of three coumarinolignoids, cleomiscosin A (Cliv A), cleomiscosin B (Cliv B) and cleomiscosin C (Cliv C) in different extracts of the seeds of Cleome viscosa using photodiode array detection at 326 nm. Cliv A, B and C were separated on a Waters symmetry C₁₈ column (250 × 4.6 mm, 5 μm) using the solvent system consisting of a mixture of acetonitrile : methanol (1:2 v/v) and water : acetic acid (99.5:0.5 v/v) as a mobile phase in a gradient elution mode. The calibration curves were linear in the concentration ranges 15–200, 10–80 and 15–180 μg/mL for Cliv A, Cliv B and Cliv C, respectively. The limits of detection and quantification for Cliv A, Cliv B and Cliv C were 15 and 20 μg/mL, 10 and 15 μg/mL and 15 and 20 μg/mL, respectively. The intra‐day and inter‐day precisions were 2.08 and 0.93% for Cliv A , 1.22 and 0.39% for Cliv B and 1.29 and 0.23 for Cliv C respectively. The developed HPLC method was used to identify and quantify Cliv A, Cliv B and Cliv C in different extracts of seed of Cleome viscosa. Copyright © 2010 John Wiley & Sons, Ltd.     

Determination of tryptophan in raw materials, rat brain and human plasma by RP-HPLC technique

This paper describes tryptophan (TRP) estimation in raw human plasma and rat brain by reversed-phase high-performance liquid chromatography (RP-HPLC). Estimation was carried out on a Purospher STAR C18 column using water-acetonitrile (90:10 v/v, at pH 2.7) mixture at a rate of 1.5 mL/min as mobile phase. Eluents were monitored at 273 nm by an ultraviolet detector. The method was linear (R(2) > 0.999), precise (intra-day and inter-day precision <2%) in the range of 0.25-20 μg/mL. The detection and quantification limits were 0.0144 μg/mL and 0.0437 μg/mL, respectively. In human plasma, Day 1 and Day 2 precision were 0.054-2.29% and 1.66-3.7%; whereas precisions in rat brain were 1.23-2.3% and 0.677-4.2%, respectively. The method was applied to study TRP level in human smokers and in arthritic rat brain. An efficient RP-HPLC method was developed for TRP determination that worked for clinical and research purposes.     

Development of method for determination and preconcentration of uranium in water samples using XAD-4 resin loaded with Br-PADAP

In the present work, a minicolumn of XAD-4 loaded with 2-(5-bromo-2-pyridylazo)-5-(diethylamino)-phenol (Br-PADAP) is proposed as a preconcentration system for uranium determination in well, tap and mineral water samples by spectrophotometer using arsenazo III as the chromogenic reagent. Initially, a two-level (2³) full factorial design was used for the preliminary evaluation of three factors, involving the following variables: sampling flow rate, elution flow rate, and pH. This design has revealed that, for the studied levels, buffer concentration and pH were significant factors. When the experimental conditions established in the optimization step were pH = 8.6, and an elution flow rate of 8.6 mL min^?1 using 0.5% m/v ascorbic acid, this system has allowed for the determination of uranium with a detection limit (LOD) (3σ/S) of 0.05 μg L^?1 and a quantification limit (LOQ) (10σ/S) of 0.16 μg L^?1. The precision expressed as the relative standard deviation (R.S.D.) of 0.8% and 1.9% at 10.0 and 1.0 μg L^?1, respectively- and a preconcentration factor of 184.5 for a sample volume of 50.0 mL. Accuracy was confirmed by uranium determination in the standard reference material, NIST SRM 1566b trace element units in Oyster Tissue samples, and spike tests with recuperations ranging from 93.2 to 105%; the procedure were applied for uranium determination in tap water, well water, and drinking water samples collected from Caetité and Cruz das Almas Cities, Bahia, Brazil. Five water samples were analyzed the uranium concentrations varied from 0.50 to 2.07 μg L^?1     

Leaching of Triazine Pesticides in Loamy Soil and their Determination by Reversed Phase HPLC

Abstract

The separation and identification of triazine pesticides (ametryn, atrazine, cyanazine and simazine) was carried out on Nova Pak C₁₈ column (150 × 3.9mm). The mobile phase used was acetonitrile-water (65:35, v/v) adjusted to pH 4.5 with acetic acid. The flow rate of the mobile phase used was 1.0mL/min. The detection of the pesticides was carried out at 250 nm. The values of the separation factor (α) were in the range of 1.49–5.32 and the values of the resolution factors (R _s) were ranged from 1.18 to 2.99 for the separated pesticides. The developed HPLC method was used to determine the concentrations of the reported pesticides in the loamy soil samples. The recovery of the pesticides from soil samples was found to be about 50%. The relative standard deviation and limit of detection were in the range of 0.01–0.02 and 0.5–1.0 μg/mL respectively.     

Determination of oleanolic and ursolic acid in Chinese herbs using HPLC and γ-CD as mobile phase modifier

To separate and determine oleanolic acid and ursolic acid, a rapid and accurate HPLC using γ‐CD as the mobile phase additive was developed. The effect of CD nature and concentration, and the acidity of the mobile phase on the chromatographic behavior of two bioactive triterpenes were systematically studied. Two bioactive triterpenes were completely separated (R = 3.11) on a Kromasil^® C₁₈ column (150×4.6 mm id, 5 μm) with the mobile phase consisting of acetonitrile/0.1% phosphoric acid with 2 mM γ‐CD as the mobile phase modifier (60:40, v/v). The flow rate was set at 1.0 mL/min and the eluent was detected at 210 nm for two bioactive triterpenes. The linearity of the method was excellent (r=0.9999) over the studied range of 6–300 μg/mL for oleanolic acid, and 12–600 μg/mL for ursolic acid. The LOD and LOQ were 1.5 and 5.0, 1.0 and 3.0 μg/mL for oleanolic acid and ursolic acid, respectively. The optimized method was successfully applied to separate and determine two bioactive triterpenes in five Chinese herbs. It is concluded that this method could be used for rapid and accurate qualitative and quantitative analysis of the two bioactive triterpenes in Chinese herbs.     

HPLC Determination of Valproic Acid in Human Serum Using Ultraviolet Detection

Abstract

A sensitive HPLC method with minimal sample preparation and good reproducibility for the determination of valproic acid in serum is described. Serum samples were precipitated using acetonitrile containing diazepam as the internal standard. Chromatography was performed on a Hewlett Packard model 1090 equipped with an octadecylsilane column and a Beckman model 163 variable wavelength detector. The drug and internal standard were eluted isocratically using a mobile phase consisting of 0.01M sodium phosphate monobasic solution, pH 2.3 and acetonitrile (63:37 v/v) followed by a gradient to flush the column before the next sample injection. The flow rate was 2.5 mL/min, the injection volume was 25 μL and the effluent was monitored at 210 nm. The serum standard curve was linear from 2.5-200.0 μg/mL with a correlation coefficient of 0.9994. Day-to-day precision for quality control samples (10.0, 25.0, 75.0 μg/mL serum) ranged from 5.6-9.6% CV. Possible interferences from other drugs which might be administered concurrently were studied. The method has been applied to the analysis of human serum samples.     

Simultaneous quantitative analysis of phosphocreatine,creatine and creatinine in plasma of children by HPLC–MS/MS method: Application to a pharmacokinetic study in children with viral myocarditis

A simple and rapid HPLC–MS/MS method was developed and validated for simultaneous measurement of phosphocreatine and its metabolites creatine and creatinine in children's plasma. A 50 μL aliquot of plasma was prepared by protein precipitation with acetonitrile–water (1000 μL, 1:1, v/v) followed by separation on a Hypersil Gold C₁₈ column (35°C) with gradient mobile phase consisting of 2 mm ammonium acetate aqueous solution (pH 10) and methanol at a flow rate of 0.3 mL/min and analyzed by mass spectrometry in both positive (phosphocreatine) and negative (creatine and creatinine) ion multiple reaction monitoring mode. Good linearity (r > 0.99) was obtained for the three analytes. The intra‐day and inter‐day values of CV were <5.46% (?13.09% ≤ RE ≤ 2.57%). The average recoveries of the three analytes were 70.9–97.5%. No obvious impact was found for the quantitation of three analytes in normal, hemolyzed and hyperlipemic plasma. In the end, this method was successfully applied to a pharmacokinetic study of phosphocreatine in children (six cases) with viral myocarditis of children after intravenous infusion of 2 g of the test drug. The pharmacokinetc parameters of phosphocreatine/creatine were as follows: t_1/2 0.24/0.83 h, T_max 0.49/0.55 h, C_max 47.34/59.29 μg/mL, AUC_last 17.07/59.63 h μg/mL, AUC_inf 17.16/79.01 h μg/mL and MRT 0.29/0.67 h.     

Sodium desoxycholate‐assisted capillary electrochromatography with methacrylate ester‐based monolithic column on fast separation and determination of coumarin analogs in Angelica dahurica extract

A rapid and sensitive CEC method with methacrylate ester‐based monolithic column has been developed for separation and determination of five coumarins (byakangelicin, oxypeucedanin hydrate, xanthotoxol, 5‐hydroxy‐8‐methoxypsoralen and bergapten) in Angelica dahurica extract. Surfactant sodium desoxycholate (SDC) was introduced into the mobile phase as the pseudostationary to dynamically increase the selectivity of analytes instead of increasing the hydrophobicity of stationary phase. In addition, other factors, pH of phosphate buffer, ACN content and applied voltage, for instance, have also an obvious effect on the resolution but little on the retention time. Satisfactory separation of these five coumarins was achieved within 6 min under a 30:70 v/v ACN–buffer containing 20 mM sodium dihydrogen phosphate (NaH₂PO₄) and 0.25 mM SDC at pH 2.51. The RSDs of intraday and interday for relative peak areas were less than 3.0% and 4.7%, respectively; and the recoveries were between 87.5% and 95.0%. The LODs were lower than 0.15 μg/mL and the LOQs were lower than 0.30 μg/mL, respectively, while calibration curves showed a good linearity (r² > 0.9979). Finally, five target coumarins from the crude extracts of A. dahurica were separated, purified, and concentrated by D‐101 macroporous resin, and were successfully separated and quantitatively determined within 6 min.     

Celecoxib determination in different layers of skin by a newly developed and validated HPLC‐UV method

A simple, rapid and sensitive analytical procedure for the measurement of celecoxib (CXB) levels in skin samples after in vitro penetration studies was developed and validated. In vitro permeability studies in porcine skin were performed for quantification of CXB at different layers of skin, the stratum corneum (SC) and epidermis plus dermis (EP + D) as well as in the acceptor solution (AS) to assess CXB permeation through skin. CXB was quantified by HPLC using a C₁₈ column and UV detection at 251 nm. The mobile phase was methanol–water 72:28 (v/v) and the flow‐rate was 0.8 mL/min. The CXB retention time was 5 min. The assay was linear for CBX in the concentration range of 0.1–3.0 μg/mL in the AS (drug permeated through skin) and 5.0–50.0 μg/mL for drug retained in SC and [EP + D] in vitro. The linear correlation coefficients for the different calibration curves were equal or greater than 0.99. Intra‐ and inter‐assay variabilities were below 8.0%. Extraction of CXB from skin samples showed recoveries higher than 95.0% after 15 min of ultrasonic sound and centrifugation at 2500 rpm for 3 min. The method was considered appropriate for the assay of CXB in skin samples, after in vitro cutaneous penetration studies. Copyright © 2011 John Wiley & Sons, Ltd.     

A new butenolide cinnamate and other biological active chemical constituents from Polygonum glabrum

Phytochemical investigation of the methanol extract of the aerial parts of Polygonum glabrum afforded one new natural product ( ? )-2-methoxy-2-butenolide-3-cinnamate (1) along with six known compounds, β-hydroxyfriedalanol (2), 3-hydroxy-5-methoxystilbene (3), ( ? ) pinocembrin (4), sitosterol-(6′-O-palmitoyl)-3-O-β-d-glucopyranoside (5), ( ? ) pinocembrin-5-methyl ether (6) and sitosterol-3-O-β-d-glucopyranoside (7). Compound 1 showed promising in vitro anti-HIV-1 activity against primary isolates HIV-1_UG070 (X4, subtype D) and HIV-1_VB59 (R5, subtype C) assayed using TZM-bl cell line with IC₅₀ in the range of 15.68–22.43 μg/mL. The extract showed TI in the range of 19.19–27.37 with IC₅₀ in the range of 10.90–15.55 μg/mL. Compounds 1, 3 and 4 exhibited in vitro anti-mycobacterium activity against Mycobacterium tuberculosis H37Ra with IC₅₀ values of 1.43, 3.33 and 1.11 μg/mL in dormant phase and 2.27, 3.33 and 1.21 μg/mL in active phase, respectively. Compound 4 was found to be the most active antiproliferative with IC₅₀ values of 1.88–11.00 μg/mL against THP-1, A549, Panc-1, HeLa and MCF7 cell lines.     

Ion‐pair cloud‐point extraction: A new method for the determination of water‐soluble vitamins in plasma and urine

A novel, simple, and effective ion‐pair cloud‐point extraction coupled with a gradient high‐performance liquid chromatography method was developed for determination of thiamine (vitamin B₁), niacinamide (vitamin B₃), pyridoxine (vitamin B₆), and riboflavin (vitamin B₂) in plasma and urine samples. The extraction and separation of vitamins were achieved based on an ion‐pair formation approach between these ionizable analytes and 1‐heptanesulfonic acid sodium salt as an ion‐pairing agent. Influential variables on the ion‐pair cloud‐point extraction efficiency, such as the ion‐pairing agent concentration, ionic strength, pH, volume of Triton X‐100, extraction temperature, and incubation time have been fully evaluated and optimized. Water‐soluble vitamins were successfully extracted by 1‐heptanesulfonic acid sodium salt (0.2% w/v) as ion‐pairing agent with Triton X‐100 (4% w/v) as surfactant phase at 50°C for 10 min. The calibration curves showed good linearity (r² > 0.9916) and precision in the concentration ranges of 1‐50 μg/mL for thiamine and niacinamide, 5–100 μg/mL for pyridoxine, and 0.5–20 μg/mL for riboflavin. The recoveries were in the range of 78.0–88.0% with relative standard deviations ranging from 6.2 to 8.2%.     

Simultaneous Determination of Nickel and cobalt in Manganese Sulphate Electrolyte by DMGH2-Sensitized Differential Pulse Polarography

Abstract

A method is described for the simultaneous determination of nickel and cobalt in manganese sulphate electrolyte by the dimethylglyoxime (DMGH₂) sensitized differential pulse polarography. The high manganese sulphate background (1.2M) in the concentrated process plant electrolyte interferes only with the nickel determination and precludes its direct determination. A 50% v/v dilution and an excessive amount (2 × 10^?3M) of the chelating agent are required at pH7.7 for the reliable determination of both elements. Under these conditions, the linear concentration ranges are 0-110 μg/1 for nickel and 0-140 μg/1 for cobalt. The minimum detectable amounts above the levels present in the process plant electrolyte are 2 μg/1 and 1 μg/1 for both elements, respectively. The relative standard deviations for all measurements are between 1 and 3%.