scholarly journals DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD FOR ISOSULFAN BLUE BY LIQUID CHROMATOGRAPHY

2017 ◽  
Vol 9 (2) ◽  
pp. 42
Author(s):  
Kishorkumar L. Mule ◽  
Dnyandeo B. Pathare
Keyword(s):  
Quantitative Determination ◽  
Analytical Method ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
Isosulfan Blue ◽  
Related Impurities ◽  
Drug Substances ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Objective: To develop and validate new, simple and rapid analytical method for determination of related impurities in isosulfan blue drug substances by the liquid chromatographic method as per ICH guidelines.Methods: The chromatographic separation obtained between drug substance i.e. isosulfan blue and its related impurities (Impurity-A, Impurity-B and Impurity-C) on C18 (100 x 2.00 mm) 1.9µ UPLC column using a mobile phase system containing 0.1 % perchloric acid in water (Mobile phase A) and 0.1 % perchloric acid in mixture of 30 volumes of water and 70 volumes of acetonitrile (Mobile Phase B) with gradient program; detector wavelength 220 nm and column temperature 30 °C. The developed method was extensively validated according to ICH guidelines.Results: Good linearity was observed for isosulfan blue, impurity-A, impurity-B and impurity-C, linearity was calculated from loq Level To 150%with respect to specification level. The correlation coefficient R = 0.999 was proved and showed that the method is robust. The limit of detection of isosulfan blue, impurity-A, impurity-B and impurity-C were found to be 0.010%, 0.015%, 0.030% and 0.0075 % respectively and limit of quantitation of isosulfan blue, impurity-A, impurity-B and impurity-C were found to be 0.030%, 0.030%, 0.045% and 0.015% respectively for 2ml injection volume. The percentage recovery of isosulfan blue and its related impurities were ranged from 94.0 to 108.0 in bulk drug samples. Isosulfan blue sample solution and mobile phase were found to be stable for at least 72 h. The proposed method was found to be suitable and accurate for the quantitative determination of impurity-A, impurity-B, impurity-C and other unknown impurities in isosulfan blue drug substances.Conclusion: A new, simple and rapid method has been developed and validated for separation and determination of impurity-A, impurity-B, impurity-C and unknown impurities of isosulfan blue by the reverse-phase liquid chromatographic method. Analytical method was developed and validated as per ICH guidelines.The developed method can be used for the quantitative determination of impurity A, impurity B, impurity C and unknown impurities in isosulfan blue drug substances in pharmaceutical industry.

A Green Liquid Chromatographic Method For The Simultaneous Determination of Chlorpheniramine Maleate, Pseudoephedrine Hydrochloride and Propyphenazone

2019 ◽  
Vol 15 (6) ◽  
pp. 635-641
Author(s):  
Nadia M. Mostafa ◽  
Ghada M. Elsayed ◽  
Nagiba Y. Hassan ◽  
Dina A. El Mously
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Dosage Form ◽  
Chromatographic Method ◽  
Green Analytical Chemistry ◽  
Chlorpheniramine Maleate ◽  
Accuracy And Precision ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Background:The concept of green analytical chemistry prevails due to the growing environmental pollution.Objective:Our attempts are to develop simple and eco-friendly method which is non-harmful to the environment by producing minimal waste. In this context, a green liquid chromatographic method was applied for the simultaneous determination of chlorpheniramine maleate, pseudoephedrine hydrochloride and propyphenazone in their combined dosage form.Methods:Separation was carried out using X select HSS RP C18 analytical column (250 × 4.6 mm, 5μm) using methanol - 0.02 M phosphate buffer pH 3 - triethylamine (60:40: 0.1, by volume) as a mobile phase. The separated peaks were detected at 215 nm at a flow rate 1.0 mL/min.Results:Quantification was done over the concentration ranges of 1-25 µg/mL for chlorpheniramine maleate, 5-35 µg/mL for pseudoephedrine hydrochloride and 10-120 µg/mL for propyphenazone. The suggested method was validated with regard to linearity, accuracy and precision according to the International Conference on Harmonization guidelines with good results.Conclusion:It could be used as a safer alternative for routine analysis of the mentioned drugs in quality control laboratories.

Validation of Liquid Chromatographic Method for Assay of Calcitriol and Alfacalcidol in Capsule Formulations

1986 ◽  
Vol 69 (6) ◽  
pp. 1026-1030
Author(s):  
Bruce C Flann ◽  
Bruce A Lodge
Keyword(s):  
Standard Deviation ◽  
Calibration Curve ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
Liquid Chromatographic Method ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic ◽  
Better Than

Abstract The validation of a liquid chromatographic procedure suitable for the determination of calcitriol and alfacalcidol in their respective formulations labeled to contain at least 0.25 μ.g drug per unit is described. The capsule content is diluted and chromatographed in 15-20 min on silica columns (5 μm) with a mobile phase of hexane-tetrahydrofuranmethylene dichloride-isopropanol (72 + 12 + 12 + 4, v/v) with detection at 254 nm. The calibration curve is linear. Recoveries of “spikes” averaged 101% with a standard deviation of 2%. Precision was better than 1.5%.

scholarly journals Development and Validation of a Liquid Chromatographic Method for the Simultaneous Determination of Estradiol, Estriol, Estrone, and Progesterone in Pharmaceutical Preparations

2009 ◽  
Vol 92 (3) ◽  
pp. 846-854 ◽  
Author(s):  
Phyllis Wilson
Keyword(s):  
Mobile Phase ◽  
Chromatographic Method ◽  
Pharmaceutical Preparations ◽  
Men And Women ◽  
Naturally Occurring ◽  
Vital Functions ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic

Abstract Progesterone and estrogens are hormones produced in the human body that are essential for regulating many vital functions. The three major estrogens produced by women are estriol, estradiol, and estrone. Progesterone is a naturally occurring hormone in both men and women. Pharmaceuticals containing estrogens alone or estrogens in combination with progesterone are commonly used in therapy. Patients requiring unique combinations of the drugs rely on pharmacies to compound the ingredients. In order to assess the potency of drugs containing combinations of estrogens and progesterone, a method was developed to determine all four ingredients simultaneously. The liquid chromatographic method utilized a Bondapak C18 column with an isocratic mobile phase of acetonitrilewater (50 + 50, v/v) at a flow rate of 1.0 mL/min and temperature of 30C. Under these conditions, the order of elution was estriol, estradiol, and estrone, followed by progesterone. UV detection was at 205 nm to monitor elution of the estrogens, then switched to 270 nm to monitor progesterone. The method was applied to the analysis of pharmacy-compounded drugs containing combinations of the hormones. Validation studies demonstrated that the method is accurate and precise.

Determination of Cymiazole Residues in Honey by Liquid Chromatography

1993 ◽  
Vol 76 (1) ◽  
pp. 92-94 ◽  
Author(s):  
Paolo Cabras ◽  
Marinella Melis ◽  
Lorenzo Spanedda
Keyword(s):  
Liquid Chromatography ◽  
Chromatographic Analysis ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
Reversed Phase ◽  
Limit Of Determination ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic ◽  
Control Samples

Abstract A liquid chromatographic method is described for the determination of cymiazole residues in honey. This acaricide is determined on a reversed-phase (C18) column, with a CH3CN-O.OOIN HCI-NaCI mixture (950 mL + 50 mL + 0.3 g/L) as the mobile phase, and UV detection at 265 nm. Cymiazole is extracted with n-hexane from aqueous alkalinized (pH 9) honey solutions. No further cleanup of the honey extract was required before chromatographic analysis. Recoveries on control samples fortified with 0.01,0.10, and 1.00 ppm cymiazole ranged from 92 to 102%. The limit of determination was 0.01 ppm.

scholarly journals New Liquid Chromatographic Method for Determination of Rabeprazole Sodium in Coated Tablets

2004 ◽  
Vol 87 (4) ◽  
pp. 842-846 ◽  
Author(s):  
Cássia V Garcia ◽  
Clésio S Paim ◽  
Martin Steppe
Keyword(s):  
Quantitative Determination ◽  
Proton Pump ◽  
Chromatographic Method ◽  
Array Detector ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Validation Parameters ◽  
Rabeprazole Sodium ◽  
Liquid Chromatographic

Abstract Rabeprazole sodium is a proton pump inhibitor that covalently binds and inactivates the gastric parietal cell proton pump (H+/K+ ATPase). Little has been published about the quantitative determination of this drug. The aim of this research was to develop a new liquid chromatographic method for quantitative determination of rabeprazole in coated tablets. The system consisted of a Hypersil Keystone Betabasic C8 column (250 × 4.6 mm, 5 μm particle size), an isocratic acetonitrile–water (35 + 65) mobile phase at a flow rate of 1.0 mL/min, and a diode array detector set at 282 nm. The following validation parameters were evaluated: linearity, precision, accuracy, specificity, detection and quantitation limits, and robustness. The method showed good linearity in the concentration range of 10–70 μg/mL. The quantitation limit was 2.43 μg/mL, and the detection limit was 0.80 μg/mL. The intra- and interday precision data showed that the method has good reproducibility (relative standard deviation = 1.03). Accuracy and robustness were also evaluated, and the results were satisfactory. The mean recovery was 101.61%. The analysis of a placebo mixture demonstrated the method is also specific.

Gas-Liquid Chromatographic Isolation, Identification, and Quantitation of Some Barbiturates, Glutethimide, and Diphenylhydantoin in Whole Blood

1972 ◽  
Vol 18 (11) ◽  
pp. 1343-1349 ◽  
Author(s):  
Rodney G Cooper ◽  
Mavis S Greaves ◽  
Goronwy Owen
Keyword(s):  
Quantitative Determination ◽  
Whole Blood ◽  
Chromatographic Method ◽  
Accurate Method ◽  
Retention Data ◽  
Qualitative And Quantitative ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic ◽  
Chromatographic Isolation

Abstract An accurate method is described for the qualitative and quantitative determination of 11 barbiturates, glutethimide, and diphenylhydantoin in a single extract obtained from 1 ml of whole blood, which is extracted with ether at pH 2 and separately but simultaneously gas-liquid chromatographed on a selective (3% OV-17) and a nonselective (5% OV-1) column. Retention data are given. Results for barbiturate obtained by the Broughton [Biochem. J.63, 207 (1956)] spectrophotometric method and this gas-liquid chromatographic method are compared. Blood from more than 30 patients has been analyzed, and data are given to illustrate some of the findings.

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