Development of Analytical Method for Determination of p-toluenesulfonylurea and its Impurities in Gliclazide Drug Substances by using HPLC

Objective: To develop and validate new, simple and rapid assay method for Prochlorperazine edisylate drug substance by UPLC as per ICH guidelines.Methods: Ultra performance liquid chromatographic method was developed, optimized and validated on Acquity UPLC by using Acquity BDH300 C4 (100 x 2.1 mm) 1.7µ column. 3.85g ammonium acetate in 1000 ml of water add 0.5 ml trifluoroacetic acid and 1 ml triethylamine (Mobile phase A): 0.5 ml trifluoroacetic acid in 1000 ml acetonitrile mobile phase (Mobile phase B) with gradient program. Detector wavelength 254 nm and column temperature 30 °C.Results: Linearity study was carried out for prochlorperazine edisylate, linearity was calculated from 80 % level to 120% with respect to specification level. The correlation coefficient (r) = 0.999 was proved that the method is robust. The resolution between known impurities and Prochlorperazine edisylate found more than 2.5, it was evident from specificity test that Prochlorperazine edisylate peak are well separated from its related impurities, hence the method is specific. Prochlorperazine edisylate sample solution and mobile phase were found to be stable for at least 3 d.Conclusion: A new, simple and rapid method has been developed and validated for assay determination of prochlorperazine edisylate in drug substance by Ultra Performance Liquid Chromatography (UPLC). The analytical method was developed and validated as per ICH guidelines. The developed method can be used for the fast assay determination of prochlorperazine edisylate drug substances in research laboratories and in the pharmaceutical industry.

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

International Journal of Applied Pharmaceutics ◽

10.22159/ijap.2017v9i2.16904 ◽

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.

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382. New Analytical Method for the Determination of PPT Levels of Isocyanates in the Workplace by Triple Quadrupole Mass Spectrometry

10.3320/1.2765525 ◽

1999 ◽

Author(s):

J. LeSage ◽

C. Ostiguy ◽

H. Tra

Keyword(s):

Mass Spectrometry ◽

Analytical Method ◽

Triple Quadrupole ◽

Quadrupole Mass ◽

Triple Quadrupole Mass Spectrometry ◽

Quadrupole Mass Spectrometry

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LUMINESCENT DETERMINATION OF SUGAR IN NATURAL HONEY

Izvestia Ufimskogo Nauchnogo Tsentra RAN ◽

10.31040/2222-8349-2020-0-4-29-32 ◽

2020 ◽

Vol 0 (4) ◽

pp. 29-32

Author(s):

B.M. GAREEV ◽

◽

A.M. ABDRAKHMANOV ◽

G.L. SHARIPOV ◽

◽

...

Keyword(s):

Quantum Dots ◽

Laboratory Test ◽

Aqueous Solutions ◽

Analytical Method ◽

Sugar Content ◽

Carbon Quantum Dots ◽

Photoluminescence Intensity ◽

Sucrose Content ◽

Natural Honey

The photoluminescence of carbon quantum dots synthesized from natural honey and mixtures of honey and sugar has been studied. An increase in the sugar content leads to a decrease in the photoluminescence intensity without changing the shape of the luminescence spectrum of these quantum dots aqueous solutions, which is associated with a decrease in the yield of their synthesis in the sugar presence. The discovered effect can be used to detect sugar in honey. When examining five different market samples of flower honey using this method, two of them showed a significant decrease in the photoluminescence intensity. A laboratory test for compliance with GOST 19792-2017 Standard requirements established an excess of the sucrose content in these samples. Luminescent determination of sugar in honey does not require complicated equipment and can be used to develop a new analytical method for determining the sugar content in counterfeit natural honey.

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