Development and Validation of a Headspace Gas Chromatographic Method for the Determination of Methyl Bromide Content in Itraconazole API

2015 ◽  
Vol 59 ◽  
pp. 160-169
Author(s):  
Mannem Durga Babu ◽  
Medikondu Kishore ◽  
K. Surendra Babu
Keyword(s):  
Methyl Bromide ◽  
Chromatographic Method ◽  
Limit Of Detection ◽  
Limit Of Quantitation ◽  
Headspace Gas ◽  
Current Article ◽  
Bulk Drug ◽  
Gas Chromatographic Method ◽  
Development And Validation

To provide quality control over the manufacture of any API, it is essential to develop highly selective analytical methods. Gas chromatography with headspace (HSGC) is widely used for the determination of residual impurities and solvents in API’s. In the current article we are reporting the development and validation of a rapid and specific Head space gas chromatographic (HSGC) method for the determination of methyl bromide in Itraconazole API. The developed method was validated in terms of specificity, linearity, precision, accuracy, limit of detection (LOD) and limit of quantitation (LOQ). The developed method was utilized for the investigation of methyl bromide content in bulk drug.

scholarly journals Determination of residual solvents in paclitaxel by headspace gas chromatography

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Khaleel Noorbasha ◽  
Abdul Rahaman Shaik
Keyword(s):  
Ethyl Acetate ◽  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Limit Of Detection ◽  
Good Resolution ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Gas Chromatographic Method ◽  
Ethyl Amine

Abstract Background A simple and sensitive gas chromatographic method was developed and validated for the simultaneous determination of methanol, ethanol, acetone, isopropyl alcohol, dichloromethane, N-hexane, ethyl acetate, tetrahydrofuran, and N,N-diisopropyl ethyl amine in Paclitaxel. A chromatographic separation was done on DB-624 column, 30 m length × 0.53 mm ID, and film thickness 3 μm, using a flame ionization detector (FID) with gradient column oven temperature program. The injection was carried out in split mode, with a split ratio of 5:1. A mixture of N-methyl-2-pyrrolidinone (contains 1% piperazine) and water in the ratio of 80:20 (v/v) was selected as a diluent to obtain good sensitivity along with the recovery. Results The developed gas chromatographic method offers symmetric peak shape, good resolution of more than 2.0 between the solvent peaks, and the relative standard deviation for replicate injections of all the solvents were found to be not more than 15.0% with reasonable retention time for all the solvents. The limit of detection for methanol, ethanol, acetone, isopropyl alcohol, dichloromethane, N-hexane, ethyl acetate, tetrahydrofuran, and N,N-diisopropyl ethyl amine was found to be 304.69 ppm, 497.98 ppm, 498.99 ppm, 504.49 ppm, 61.81 ppm, 30.07 ppm, 505 ppm, 73.05 ppm, and 2.09 ppm, respectively. Limit of quantitation of methanol, ethanol, acetone, isopropyl alcohol, dichloromethane, N-hexane, ethyl acetate, tetrahydrofuran, and N,N-diisopropyl ethyl amine was found to be 89.62 ppm, 146.47 ppm, 146.76 ppm, 148.38 ppm, 18.18 ppm, 8.84 ppm, 148.53 ppm, 21.49 ppm, and 0.62 ppm, respectively. Precision was found to be satisfactory. Linear in the range of LOQ to 150% level for all the solvents, and accuracy along with robustness, is performed, and acceptable results were obtained. Conclusion The proposed method was demonstrated to be simple, sensitive, specific, linear, precise, accurate, and robust, hence can be used to determine the residual organic solvents in Paclitaxel drug substance and drug product.

Headspace Gas Chromatographic Method for Determination of Methyl Bromide in Food Ingredients

1985 ◽  
Vol 68 (6) ◽  
pp. 1112-1116
Author(s):  
Jonathan W DeVries ◽  
James M Broge ◽  
John P Schroeder ◽  
Raymond H Bowers ◽  
Paul A Larson ◽  
...  
Keyword(s):  
Detection Limit ◽  
Methyl Bromide ◽  
Chromatographic Method ◽  
Equilibration Time ◽  
Gas Chromatograph ◽  
Food Ingredients ◽  
Headspace Gas ◽  
The Matrix ◽  
Gas Chromatographic Method

Abstract A headspace gas chromatographic (GC) method, which can be automated, has been developed for determination of methyl bromide. This method has been applied to wheat, flour, cocoa, and peanuts. Samples to be analyzed are placed in headspace sample vials, water is added, and the vials are sealed with Teflon-lined septa. After an appropriate equilibration time at 32°C, the samples are analyzed within 10 h. A sample of the headspace is withdrawn and analyzed on a gas chromatograph equipped with an electron capture detector (ECD). Methyl bromide levels were quantitated by comparison of peak area with a standard. The standard was generated by adding a known amount of methyl bromide to a portion of the matrix being analyzed and which was known to be methyl bromide free. The detection limit of the method was 0.4 ppb. The coefficient of variation (CV) was 6.5% for wheat, 8.3% for flour, 3.3% for cocoa, and 11.6% for peanuts.

Determination of Residual Ethylene Oxide in Spectinomycin Hydrochloride Bulk Drug by Dynamic Headspace Gas Chromatography

1993 ◽  
Vol 76 (2) ◽  
pp. 313-319
Author(s):  
Tore Ramstad ◽  
Lisa S Miller ◽  
Virginia N Thomas
Keyword(s):  
Detection Limit ◽  
Ethylene Oxide ◽  
Chromatographic Method ◽  
Headspace Gas Chromatography ◽  
Dynamic Headspace ◽  
Relative Standard ◽  
Headspace Gas ◽  
Bulk Drug ◽  
Gas Chromatographic Method

Abstract A dynamic headspace gas chromatographic method was developed for the determination of residual ethylene oxide (EtO) in a pharmaceutical bulk drug, spectinomycin hydrochloride. The recommended column is PoraPLOT Q; PoraPLOT U was demonstrated to be equivalent. A detection limit of 2 ppb was achieved, and linearity was established to the highest value tested (5 ppm). The detection limit was 2-3 orders of magnitude lower than that achieved in previously published methods for EtO in pharmaceutical bulk drugs. Precision studies yielded relative standard deviations ranging from 2 to 10% over the 10-575 ppb concentration range. The method was applied to support EtO sterilization studies conducted at The Upjohn Company and was implemented for routine use. The sterilization studies demonstrated that residual levels of EtO <10 ppb are achievable.

Automated Closed-System Headspace Determination of Methyl Bromide in a Variety of Raw and Processed Nuts

1992 ◽  
Vol 75 (2) ◽  
pp. 328-333
Author(s):  
Joseph H Ford ◽  
Michael G Legendre ◽  
Dorothy L Ladner ◽  
Joseph A Dawson ◽  
Caleph Raymond
Keyword(s):  
Stainless Steel ◽  
Closed System ◽  
Methyl Bromide ◽  
Chromatographic Method ◽  
P Values ◽  
Headspace Gas ◽  
Different Types ◽  
Partitioning Coefficients ◽  
Gas Chromatographic Method

Abstract An automatic gas chromatographic method was developed for determining methyl bromide residues In 11 different types of nuts. A 50 g sample Is placed In a modified stainless steel blender container and mixed with 200 mL 0.5M sodium sulfate. The blender container Is sealed with a screw lid, and the sample Is blended 3 min and equilibrated 17 mln in a bath-reclrculator at 26°C. The headspace gas Is automatically sampled and analyzed twice for methyl bromide residues. Recoveries are based on deviation from predetermined partitioning coefficients (p-values). The average p-values for the different nuts ranged from 0.28 to 0.43, and the CVs for their determinations ranged from 7.7 to 23.5%. The method Is sensitive, simple, and reproducible, and It is operated In a totally closed system. Over 1100 samples of assorted nuts were analyzed within a 6-month period

A Headspace Gas Chromatographic Method for Determination of Formic acid Content in Isosulfan Blue and in Various Drugs

2021 ◽  
Vol 37 (2) ◽  
pp. 321-329
Author(s):  
Nilesh Takale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Rajarajan Govindasamy
Keyword(s):  
Sulfuric Acid ◽  
Formic Acid ◽  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Class Iii ◽  
Drug Substances ◽  
Headspace Gas ◽  
Concentrated Sulfuric Acid ◽  
Gas Chromatographic Method

The Pharmaceutical industry uses formic acid in the manufacturing of various drug substances or API. At the time of manufacturing of API formic acid is use as an oxidizing agent. Formic acid is the simplest carboxylic acid. It also called methanoic acid.Formic acid present in API at high concentrations is very hazardous but in low concentrations is very beneficial. The developed and validated method was short, precise, cost effective and reproducible with FID detector and easy to use. The method is a selective and superficial analytical method for determination of formic acid in different drug substances. We report here the development and validation study of headspace gas chromatographic method to determine formic acid in different drug substances we are reported here. As per this method, the drug sample was dissolved in 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol (IPA) in a GC headspace vial and 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol used as a diluent. A AB-Inowax capillary column (30 m x 0.32 mm I.D. and 0.5 µm film thickness) was used under gradient conditions with FID. The formic acid peak was well separated from all other solvents that are used in synthesis of particular drug substance. The LOD and LOQof the method for formic acid are 82 ppm and 249 ppm respectively. Formic acid are low toxic class-III solvent as per ICH guideline.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING HPTLC METHOD FOR DETERMINATION OF APIXABAN AS BULK DRUG

2019 ◽  
pp. 37-42
Author(s):  
Mrinalini C. Damle ◽  
Swapnil S Waghmare ◽  
PURUSHOTAM SINHA
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Limit Of Detection ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Chromatographic Condition ◽  
Bulk Drug ◽  
Development And Validation ◽  
Hptlc Method

Objective: To develop and validate simple, sensitive stability indicating HPTLC (High performance thin layer chromatography) method for apixaban. Methods: The chromatographic separation was performed on aluminium plates precoated with silica gel 60 F254 using toluene: ethyl acetate: methanol (3:6:1 v/v/v) as mobile phase followed by densitometric scanning at 279 nm. Results: The chromatographic condition shows sharp peak of apixaban at Rf value of 0.38±0.03. Stress testing was carried out according to international conference on harmonization (ICH)Q1A (R2) guidelines and the method was validated as per ICH Q2(R1) guidelines. The calibration curve was found to be linear in the concentration range of 100-500 ng/band for apixaban. The limit of detection and quantification was found to be 11.66ng/bandand35.33ng/band, respectively. Conclusion: A new simple, sensitive, stability indicating high performance thin layer chromatographic (HPTLC) method has been developed and validated for the determination of apixaban.

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