Validation of an analytical method for quality control of residual solvents (n-hexane and acetone) in D-002: New active ingredient from beeswax

Antolín, Ernesto Méndez; Quiñónez, Yaisme Balcinde; Canavaciolo, Víctor González; Cruz, Esperanza Rodríguez

doi:10.1016/j.jpba.2008.02.003

Cited by 14 publications

(6 citation statements)

References 5 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…In the case of the analyses using HS-GC/MS, the recoveries and CV of the N,N-dimethylacetamide solvent were 96.39-119.86 and 0.04-1.25%, respectively, and those of the benzyl alcohol solvent were 95.96-115.63 and 0.19-11.6%, respectively. Antolín et al (4) reported mean recoveries±SD of 92.3±15.4-108.6±15.8% for the analysis of residual n-hexane in the active ingredient of beeswax using HS-GC/FID. Ramos (15) reported that the recoveries for the analysis of the residual hexane in five drug substances using HS-GC equipped with FID were 98.5-103.2% for the range of 463-831 ppm.…”

Section: Methods Validation For Hexane Analysismentioning

confidence: 99%

“…A number of studies have been performed previously on the analysis of hexane in food products. A method to analyze the residual hexane in vegetable oil (3), beeswax (4), annatto extracts (5), and drug substance (6) was developed using headspace gas chromatography (GC). A method to analyze the residual hexane in olive oil (7) was developed using headspace-solid phase microextraction (SPME).…”

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

An analysis method for determining residual hexane in health functional food products using static headspace gas chromatography

Jeong

Lee

Kim

et al. 2017

Food Sci Biotechnol

View full text Add to dashboard Cite

A method for analyzing the contents of residual hexane in health functional food products was developed. The dissolving solvents in the health functional food products and the internal standard selected were -dimethylacetamide and heptane, respectively. The analysis conditions for headspace-gas chromatography/flame ionization detection (HS-GC/FID) and headspace-gas chromatography/mass spectrometry (HS-GC/MS) were determined as 18 mL of headspace volume, 100°C of headspace oven temperature, and 30 min of equilibration time; a Durabond (DB)-624 column was selected for this analysis. To validate this method, which applies N,N-dimethylacetamide as a dissolving solvent, the limit of detection and limit of quantification (LOQ) values based on the HS-GC/FID and HS-GC/MS analyses results were found to be 0.10, 0.29 and 0.16, 0.47 mg/L, respectively. The recoveries and coefficient of variation (CV) obtained by HS-GC/MS were 96.39-119.86% and 0.04-1.25%, respectively, better than those obtained by HS-GC/FID. By applying the HS-GC/MS method, it was possible to analyze the content of the residual hexane in 60 different types of health functional food products.

show abstract

Section: Methods Validation For Hexane Analysismentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

An analysis method for determining residual hexane in health functional food products using static headspace gas chromatography

Jeong

Lee

Kim

et al. 2017

Food Sci Biotechnol

View full text Add to dashboard Cite

show abstract

“…Residual solvents or volatile organic solvents are used or formed during the manufacturing of pharmaceutical drug substances, intermediates, excipients or pharmaceutical drug product [1]. The solvents are toxic, have no therapeutic importance and affect the quality and stability of drug substances and drug products so they are not desirable in the final product [2][3][4]. Although it is difficult to remove completely with the common techniques used in practical manufacturing process such as increased process temperature or/and decreased pressure, they need to be minimized.…”

Section: Introductionmentioning

confidence: 99%

Development and validation of residual solvent determination by headspace gas chromatography in Imatinib Mesylate API

et al. 2019

View full text Add to dashboard Cite

An accurate, precise, robust and sensitive method was developed for residual solvents determination by fast static headspace gas chromatography (HSGC) with flame ionization detector in Imatinib Mesylate API. Residual solvents in drug substances are quantified using gas chromatography with headspace. As per regulatory guidelines, residual solvents must be controlled for release any batches of active pharmaceutical ingredients (API). This paper includes the development and validation of HSGC method for the determination of residual solvents specifically methanol, acetone, dichloromethane, n-hexane, ethyl acetate and pyridine in Imatinib Mesylate API. Imatinib Mesylate is a specific inhibitor of BCR-ABL tyrosine kinase. DB-624 capillary column, 30 m long × 0.53 mm internal diameter, the 3 µm film thickness was used for analysis. To minimize degradation, injector temperature was set at 170 °C. The initial oven temperature was kept at 35 °C for 2 min and used ramp 1 at a rate of 4 °C min −1 to temperature of 80 °C hold for 0 min and used ramp 2 at a rate of 40 °C min −1 to a final temperature of 230 °C for 12 min hold time. Nitrogen was selected as a carrier gas. 1-Methyl-2-Pyrrolidinone (NMP) was used as a sample solvent. The method can be readily used to determine defined residual solvents present in a various range of APIs, intermediates, excipients and drug products.

show abstract

“…The European Union (EU) Community has set 1 mg/kg of hexane residue in vegetable oils (8). Several studies estimated hexane residue in vegetable oil (9), beeswax (10), annatto extracts (11) using headspace gas chromatography (GC). Michulec et al (2004) evaluated the presence of hexane, benzene and toluene in the vegetable oils, cardamom and vitamin A using HS-GC-FID (12).…”

Section: Introductionmentioning

confidence: 99%

Evaluation of Hexane Content in Edible Vegetable Oils Consumed in Iran

Yousefi

Hosseini

2017

JECT

View full text Add to dashboard Cite

Solvent residue such as hexane in foodstuff, especially edible oil could be considered as the undesirable substances when exceeds maximum residue limit (MRL). The aim of this study is to determine the hexane content in various brands of edible oils. Totally forty samples (23 brands) of different types of vegetable oils including frying oils (n=14), blended oils (n=13), sunflower oils (n=6), corn oils (n=5) and canola oils (n=2) from Iran´s market were analyzed for hexane content using solid phase microextraction gas chromatography equipped with a flame-ionization detector (SPME)-GC-(FID). The hexane residue was detected in thirty-six out of forty examined samples, ranged from lower than LOD to 42.6 µg/kg. However, in all of them hexane content were below the MRL of 1 mg/kg which set by the European Union.

show abstract

Validation of an analytical method for quality control of residual solvents (n-hexane and acetone) in D-002: New active ingredient from beeswax

Cited by 14 publications

References 5 publications

An analysis method for determining residual hexane in health functional food products using static headspace gas chromatography

An analysis method for determining residual hexane in health functional food products using static headspace gas chromatography

Development and validation of residual solvent determination by headspace gas chromatography in Imatinib Mesylate API

Evaluation of Hexane Content in Edible Vegetable Oils Consumed in Iran

Contact Info

Product

Resources

About