Development and Validation of a Procedure for the Quantitative Determination of Residual Organic Solvents in Allergen Preparations by GC
Introduction. One of the requirements for the quality of pharmaceuticals, including allergens, is the determination of residual organic solvents in them. In the production of allergen preparations, in a number of cases in the technological process, organic solvents of the third toxicity class are us...
| Main Authors: | , , , , , , , , |
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| Format: | Article |
| Language: | Russian |
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LLC Center of Pharmaceutical Analytics (LLC «CPHA»)
2022-05-01
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| Series: | Разработка и регистрация лекарственных средств |
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| Online Access: | https://www.pharmjournal.ru/jour/article/view/1230 |
| _version_ | 1797874878141956096 |
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| author | R. A. Bubenchikov E. I. Sakanyan N. V. Zubkova V. P. Dobrynin S. V. Goriainov F. Hajjar E. A. Platonov D. I. Pisarev R. A. Abramovich |
| author_facet | R. A. Bubenchikov E. I. Sakanyan N. V. Zubkova V. P. Dobrynin S. V. Goriainov F. Hajjar E. A. Platonov D. I. Pisarev R. A. Abramovich |
| author_sort | R. A. Bubenchikov |
| collection | DOAJ |
| description | Introduction. One of the requirements for the quality of pharmaceuticals, including allergens, is the determination of residual organic solvents in them. In the production of allergen preparations, in a number of cases in the technological process, organic solvents of the third toxicity class are used, diethyl ether and acetone, which are solvents of low toxicity and their maximum content is allowed up to 0.5 % (5000 ppm). Since diethyl ether or acetone, and in some cases both solvents can be used simultaneously in the production process of allergen preparations for degreasing and cleaning, it is therefore advisable to develop and use a unified technique to determine them.Aim. The aim of the study was to develop and validate a method for the quantitative determination of residual organic solvents in allergen preparations.Materials and methods. The studies were carried out by gas-liquid chromatography with a flame ionization detector with injection of the test samples using an autosampler on a Zebron ZB-624 capillary quartz column (G43, 6 % cyanopropylphenyl / 94 % dimethylpoly siloxane).Results and discussion. The conditions for the chromatographic separation of acetone and diethyl ether on a capillary quartz column were selected. The parameters of the suitability of the chromatographic system have been determined. The developed method was validated according to the following characteristics: specificity, linearity, limit of quantitative determination, correctness and precision at the level of repeatability and intra-laboratory precision. The content of acetone and diethyl ether in 26 preparations of allergens was determined. The results of the quantitative determination of diethyl ether and acetone in allergen preparations, in the technological process of which OOP are used, are in the range of 0.0053–0.0524 % for diethyl ether and 0.0029–0.0994 % for acetone. Thus, the content of diethyl ether and acetone in all tested allergen preparations was below the established norm (less than 0.5 %).Conclusion. An analytical method has been developed for determining the quantitative content of diethyl ether and acetone in allergen preparations using the GLC method; the method has been validated according to characteristics that meet the requirements of General Pharmacopoeia Monograph 1.1.0012.15 "Validation of analytical methods". The analysis of allergen preparations was carried out in accordance with the methodology. In all preparations, the content of diethyl ether and acetone was no more than 0.5 %. |
| first_indexed | 2024-04-10T01:38:58Z |
| format | Article |
| id | doaj.art-456583bd147f4b38aeccc2b47bb374d1 |
| institution | Directory Open Access Journal |
| issn | 2305-2066 2658-5049 |
| language | Russian |
| last_indexed | 2024-04-10T01:38:58Z |
| publishDate | 2022-05-01 |
| publisher | LLC Center of Pharmaceutical Analytics (LLC «CPHA») |
| record_format | Article |
| series | Разработка и регистрация лекарственных средств |
| spelling | doaj.art-456583bd147f4b38aeccc2b47bb374d12023-03-13T09:14:03ZrusLLC Center of Pharmaceutical Analytics (LLC «CPHA»)Разработка и регистрация лекарственных средств2305-20662658-50492022-05-0111215916810.33380/2305-2066-2022-11-2-159-168968Development and Validation of a Procedure for the Quantitative Determination of Residual Organic Solvents in Allergen Preparations by GCR. A. Bubenchikov0E. I. Sakanyan1N. V. Zubkova2V. P. Dobrynin3S. V. Goriainov4F. Hajjar5E. A. Platonov6D. I. Pisarev7R. A. Abramovich8АО «НПО «Микроген»АО «НПО «Микроген»АО «НПО «Микроген»АО «НПО «Микроген»ФГАОУ ВО «Российский университет дружбы народов» (Российский университет дружбы народов, РУДН)ФГАОУ ВО «Российский университет дружбы народов» (Российский университет дружбы народов, РУДН)ФГАОУ ВО «Российский университет дружбы народов» (Российский университет дружбы народов, РУДН)ФГАОУ ВО «Российский университет дружбы народов» (Российский университет дружбы народов, РУДН)ФГАОУ ВО «Российский университет дружбы народов» (Российский университет дружбы народов, РУДН)Introduction. One of the requirements for the quality of pharmaceuticals, including allergens, is the determination of residual organic solvents in them. In the production of allergen preparations, in a number of cases in the technological process, organic solvents of the third toxicity class are used, diethyl ether and acetone, which are solvents of low toxicity and their maximum content is allowed up to 0.5 % (5000 ppm). Since diethyl ether or acetone, and in some cases both solvents can be used simultaneously in the production process of allergen preparations for degreasing and cleaning, it is therefore advisable to develop and use a unified technique to determine them.Aim. The aim of the study was to develop and validate a method for the quantitative determination of residual organic solvents in allergen preparations.Materials and methods. The studies were carried out by gas-liquid chromatography with a flame ionization detector with injection of the test samples using an autosampler on a Zebron ZB-624 capillary quartz column (G43, 6 % cyanopropylphenyl / 94 % dimethylpoly siloxane).Results and discussion. The conditions for the chromatographic separation of acetone and diethyl ether on a capillary quartz column were selected. The parameters of the suitability of the chromatographic system have been determined. The developed method was validated according to the following characteristics: specificity, linearity, limit of quantitative determination, correctness and precision at the level of repeatability and intra-laboratory precision. The content of acetone and diethyl ether in 26 preparations of allergens was determined. The results of the quantitative determination of diethyl ether and acetone in allergen preparations, in the technological process of which OOP are used, are in the range of 0.0053–0.0524 % for diethyl ether and 0.0029–0.0994 % for acetone. Thus, the content of diethyl ether and acetone in all tested allergen preparations was below the established norm (less than 0.5 %).Conclusion. An analytical method has been developed for determining the quantitative content of diethyl ether and acetone in allergen preparations using the GLC method; the method has been validated according to characteristics that meet the requirements of General Pharmacopoeia Monograph 1.1.0012.15 "Validation of analytical methods". The analysis of allergen preparations was carried out in accordance with the methodology. In all preparations, the content of diethyl ether and acetone was no more than 0.5 %.https://www.pharmjournal.ru/jour/article/view/1230препараты аллергеновостаточные органические растворителигазо-жидкостная хроматографиявалидация |
| spellingShingle | R. A. Bubenchikov E. I. Sakanyan N. V. Zubkova V. P. Dobrynin S. V. Goriainov F. Hajjar E. A. Platonov D. I. Pisarev R. A. Abramovich Development and Validation of a Procedure for the Quantitative Determination of Residual Organic Solvents in Allergen Preparations by GC Разработка и регистрация лекарственных средств препараты аллергенов остаточные органические растворители газо-жидкостная хроматография валидация |
| title | Development and Validation of a Procedure for the Quantitative Determination of Residual Organic Solvents in Allergen Preparations by GC |
| title_full | Development and Validation of a Procedure for the Quantitative Determination of Residual Organic Solvents in Allergen Preparations by GC |
| title_fullStr | Development and Validation of a Procedure for the Quantitative Determination of Residual Organic Solvents in Allergen Preparations by GC |
| title_full_unstemmed | Development and Validation of a Procedure for the Quantitative Determination of Residual Organic Solvents in Allergen Preparations by GC |
| title_short | Development and Validation of a Procedure for the Quantitative Determination of Residual Organic Solvents in Allergen Preparations by GC |
| title_sort | development and validation of a procedure for the quantitative determination of residual organic solvents in allergen preparations by gc |
| topic | препараты аллергенов остаточные органические растворители газо-жидкостная хроматография валидация |
| url | https://www.pharmjournal.ru/jour/article/view/1230 |
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