Static headspace gas chromatographic method for quantitative determination of residual solvents in pharmaceutical drug substances according to European Pharmacopoeia requirements

Rial-Otero, R.; Carrera, Guillem; Dulsat, J.F.; Fábregas, José Luís; Claramunt, Juan

doi:10.1016/j.chroma.2004.09.023

Cited by 56 publications

(28 citation statements)

References 7 publications

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“…Determination of ethanol concentration was conducted according to the method of Otero et al 9 with modification. One ml of Ou saturated with sodium chloride was put into a 20-ml headspace vial with 50 µl of 1,4-dioxane added as an internal standard.…”

Section: Determination Of Ethanol By Static Headspace Techniquementioning

confidence: 99%

Volatile flavour compounds analysis of solid state fermented Thai rice wine (Ou)

Chuenchomrat¹,

Assavanig²,

Lertsiri³

2008

ScienceAsia

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Solid-state fermented Thai rice wines (Ou) were analysed to determine their chemical components. Determined parameters were pH (4.5-5.5), protein (0.45-0.99 g/100g), ash (0.10-0.30 g/100g), total solid (1.72-14.34 g/100g), glucose (4.07-7.91 mg/ml) contents and volatile compounds. The ethanol concentration was in the range of 12.15 to 104.60 mg/ml. Profiles of volatile compounds were analysed by dynamic headspace coupled with gas chromatography mass spectrometry and gas chromatography olfactometry. The potent odours were alcoholic and solvent-like, sweet, fruity, buttery, and pungent aromas. The concentration in Ou of n-propanol, iso-butyl alcohol, iso-amyl alcohol, furfuryl alcohol, benzene ethanol, acetol, 2,3-butanediol, glycerol, ethyl lactate, acetoin, furfural, 5-methyl furfural, 5-hydroxymethyl-2-furfural, and acetic acid were also determined by a direct injection technique. From principal component analysis, Ou samples could be categorized into two groups based on the concentration of ethanol and their profiles of volatile compounds.

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Section: Determination Of Ethanol By Static Headspace Techniquementioning

confidence: 99%

Volatile flavour compounds analysis of solid state fermented Thai rice wine (Ou)

Chuenchomrat¹,

Assavanig²,

Lertsiri³

2008

ScienceAsia

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“…The aim of this study is to develop and validate the GC-HS method of analysis for residual solvents namely acetone, ethyl acetate and acetonitrile in Neostigmine methylsulfate. Some of the methods for identification of residual solvent in drugs are also discussed [5][6][7][8][9]. Materials:-Reagent and Chemicals:-Neostigmine Methylsulfate sample was received from Analytical research and development department of Indoco research centre (Navi Mumbai).…”

Section: Issn: 2320-5407mentioning

confidence: 99%

Determination of Residual Solvents in Neostigmine Methylsulfate by Headspace Gas Chromatography.

Hussain¹,

Gosar²,

Shaikh³

2017

IJAR

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“…The US Pharmacopeia (USP) General Chapter Residual solvents (467), based on the European Pharmacopeia (EP) procedure [9], presented an HSGC method for testing procedures for residual solvents in pharmaceuticals. Interestingly, the procedures can be divided into two categories on the basis of the solubility of the samples: water-soluble materials and water-insoluble materials [10,11].…”

Section: Introductionmentioning

confidence: 99%

“…The HSGC method using DMF as the sample diluent has a higher precision than when water is used in the quantification of residual solvents in drug substances [12]. In the JECFA specification of bixin-based products, DMF is designated as the solvent to dissolve and dilute samples in high-performance liquid chromatography (HPLC) analysis for impurities [9]. Therefore, we thought that DMF could become a suitable sample diluent for HSGC analysis of annatto extracts.…”

Section: Introductionmentioning

confidence: 99%

Analysis of Residual Solvents in Annatto Extracts Using a Static Headspace Gas Chromatography Method

Itô¹,

Ishizuki²,

Sekiguchi³

et al. 2012

AJAC

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An analytical method for the quantification of residual solvents in annatto extracts, natural food colorants, was established using a static headspace gas chromatography (HSGC) coupled with a flame ionization detector (FID). As a sample diluent in a headspace sampling, dimethylformamide (DMF) was selected owing to its high capacity for dissolving both bixin-based and norbixin-based annatto extracts. The quantification of residual solvents was performed using the external standard method. The linearity of the calibration curves was assured with relative coefficients (R 2 ) that were greater than 0.999. The recoveries of all standard solvents spiked in the annatto extracts were in the range from 95.1% to 107.1% to verify the accuracy and the relative standard deviation (RSD%) values (n = 3) were in the range from 0.57% to 3.31%. The quantification limits (QL) were sufficiently lower than the limits specified by Joint FAO/WHO Expert Committee on Food Additives (JECFA). With the established HSGC method, six residual solvents (methanol, ethanol, 2-propanol, acetone, ethyl acetate, and hexane) in 23 commercial annatto-extract products that consist of seven bixin-based and 16 norbixin-based products were quantified. The levels of residual ethyl acetate and hexane in all products were lower than the specified limits of JECFA. However, three samples of bixin-based products showed higher levels of residual 2-propanol (approximately 313.9 -427.7 ppm) than the specified limit. Other bixin products also showed higher concentrations of residual methanol (approximately 166.6 -394.7 ppm) and residual acetone (approximately 75.2 -179.8 ppm) than the limits of JECFA. In the case of norbixin-based products, nine samples showed higher levels of residual acetone (approximately 42.6 -139.5 ppm) than the limits of JECFA. This is the first survey of residual solvents in annatto extracts using the validated HSGC method.

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Static headspace gas chromatographic method for quantitative determination of residual solvents in pharmaceutical drug substances according to European Pharmacopoeia requirements

Cited by 56 publications

References 7 publications

Volatile flavour compounds analysis of solid state fermented Thai rice wine (Ou)

Volatile flavour compounds analysis of solid state fermented Thai rice wine (Ou)

Determination of Residual Solvents in Neostigmine Methylsulfate by Headspace Gas Chromatography.

Analysis of Residual Solvents in Annatto Extracts Using a Static Headspace Gas Chromatography Method

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