Development and Validation of an Analytical Procedure for Determining Convallatoxin in Medicinal Products Containing Cardiac Glycosides of Lily of the Valley
INTRODUCTION. The safe use of lily-of-the-valley medicinal products requires adequately controlling the content of cardiac glycosides. The State Pharmacopoeia of the Russian Federation stipulates that the content of cardiac glycosides in lily-of-the-valley medicinal products should be quantified usi...
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| Format: | Article |
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Federal State Budgetary Institution ‘Scientific Centre for Expert Evaluation of Medicinal Products’ of the Ministry of Health of the Russian Federation (FSBI ‘SCEEMP’)
2024-11-01
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| Series: | Регуляторные исследования и экспертиза лекарственных средств |
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| Online Access: | https://www.vedomostincesmp.ru/jour/article/view/714 |
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| author | T. A. Golomazova N. P. Antonova N. E. Semenova E. P. Shefer S. S. Prokhvatilova |
| author_facet | T. A. Golomazova N. P. Antonova N. E. Semenova E. P. Shefer S. S. Prokhvatilova |
| author_sort | T. A. Golomazova |
| collection | DOAJ |
| description | INTRODUCTION. The safe use of lily-of-the-valley medicinal products requires adequately controlling the content of cardiac glycosides. The State Pharmacopoeia of the Russian Federation stipulates that the content of cardiac glycosides in lily-of-the-valley medicinal products should be quantified using bioassays and spectrophotometry. However, the determination of cardiac glycosides needs more accurate and selective physicochemical methods, such as high-performance liquid chromatography (HPLC).AIM. This study aimed to develop and validate an HPLC analytical procedure for the quantitative determination of cardiac glycosides (convallatoxin) in lily-of-the-valley herbal medicinal products.MATERIALS AND METHODS. The study examined the Lily-of-the-Valley Tincture, Zelenin Drops, Valocormid, Carniland®, and Lily-of-the-Valley Extract Reference Standard samples. The content of cardiac glycosides was determined by comparison with a reference standard for convallatoxin by HPLC and spectrophotometry. The samples were prepared as outlined in Monograph 3.4.0003.18 Lily-of-the-Valley Herb Tincture of the State Pharmacopoeia of the Russian Federation. Mixed cardiac glycosides were separated on a Luna 5 µm C18(2) column by gradient elution with 0.1% orthophosphoric acid in water and acetonitrile. The analysis was performed using an autoinjector with sample cooling to 5 °C.RESULTS. The developed analytical procedure met the acceptance criteria for specificity, intermediate precision, linearity (correlation coefficient of 0.99985), and repeatability (relative standard deviation of convallatoxin measurements of 1.61%). The analytical procedure is suitable for the quantitative determination of convallatoxin in lily-of-the-valley herbal medicinal products because it produces reliable and repeatable results.CONCLUSIONS. The authors developed a highly sensitive and selective HPLC analytical procedure for the quantitative determination of convallatoxin in lily-of-the-valley herbal medicinal products. The content of convallatoxin ranged from 0.012 to 0.018 mg/mL in the liquid active substance Lily-of-the-Valley Tincture, from 0.004 to 0.013 mg/mL in the medicinal product Zelenin Drops, and from 0.005 to 0.007 mg/mL in the medicinal products Carniland® and Valocormid. For the Lily-of-the-Valley Extract Reference Standard, the content of convallatoxin amounted to 0.029 mg/mL. |
| format | Article |
| id | doaj-art-e3db2c025810466d8a427c489d9529e7 |
| institution | Kabale University |
| issn | 3034-3062 3034-3453 |
| language | Russian |
| publishDate | 2024-11-01 |
| publisher | Federal State Budgetary Institution ‘Scientific Centre for Expert Evaluation of Medicinal Products’ of the Ministry of Health of the Russian Federation (FSBI ‘SCEEMP’) |
| record_format | Article |
| series | Регуляторные исследования и экспертиза лекарственных средств |
| spelling | doaj-art-e3db2c025810466d8a427c489d9529e72025-08-20T03:57:31ZrusFederal State Budgetary Institution ‘Scientific Centre for Expert Evaluation of Medicinal Products’ of the Ministry of Health of the Russian Federation (FSBI ‘SCEEMP’)Регуляторные исследования и экспертиза лекарственных средств3034-30623034-34532024-11-0114558058910.30895/1991-2919-2024-14-5-580-589473Development and Validation of an Analytical Procedure for Determining Convallatoxin in Medicinal Products Containing Cardiac Glycosides of Lily of the ValleyT. A. Golomazova0N. P. Antonova1N. E. Semenova2E. P. Shefer3S. S. Prokhvatilova4Scientific Centre for Expert Evaluation of Medicinal ProductsScientific Centre for Expert Evaluation of Medicinal ProductsScientific Centre for Expert Evaluation of Medicinal ProductsScientific Centre for Expert Evaluation of Medicinal ProductsScientific Centre for Expert Evaluation of Medicinal ProductsINTRODUCTION. The safe use of lily-of-the-valley medicinal products requires adequately controlling the content of cardiac glycosides. The State Pharmacopoeia of the Russian Federation stipulates that the content of cardiac glycosides in lily-of-the-valley medicinal products should be quantified using bioassays and spectrophotometry. However, the determination of cardiac glycosides needs more accurate and selective physicochemical methods, such as high-performance liquid chromatography (HPLC).AIM. This study aimed to develop and validate an HPLC analytical procedure for the quantitative determination of cardiac glycosides (convallatoxin) in lily-of-the-valley herbal medicinal products.MATERIALS AND METHODS. The study examined the Lily-of-the-Valley Tincture, Zelenin Drops, Valocormid, Carniland®, and Lily-of-the-Valley Extract Reference Standard samples. The content of cardiac glycosides was determined by comparison with a reference standard for convallatoxin by HPLC and spectrophotometry. The samples were prepared as outlined in Monograph 3.4.0003.18 Lily-of-the-Valley Herb Tincture of the State Pharmacopoeia of the Russian Federation. Mixed cardiac glycosides were separated on a Luna 5 µm C18(2) column by gradient elution with 0.1% orthophosphoric acid in water and acetonitrile. The analysis was performed using an autoinjector with sample cooling to 5 °C.RESULTS. The developed analytical procedure met the acceptance criteria for specificity, intermediate precision, linearity (correlation coefficient of 0.99985), and repeatability (relative standard deviation of convallatoxin measurements of 1.61%). The analytical procedure is suitable for the quantitative determination of convallatoxin in lily-of-the-valley herbal medicinal products because it produces reliable and repeatable results.CONCLUSIONS. The authors developed a highly sensitive and selective HPLC analytical procedure for the quantitative determination of convallatoxin in lily-of-the-valley herbal medicinal products. The content of convallatoxin ranged from 0.012 to 0.018 mg/mL in the liquid active substance Lily-of-the-Valley Tincture, from 0.004 to 0.013 mg/mL in the medicinal product Zelenin Drops, and from 0.005 to 0.007 mg/mL in the medicinal products Carniland® and Valocormid. For the Lily-of-the-Valley Extract Reference Standard, the content of convallatoxin amounted to 0.029 mg/mL.https://www.vedomostincesmp.ru/jour/article/view/714cardiac glycosidesconvallatoxinhigh-performance liquid chromatographyhplclily-of-the-valley herbherbal medicinal productszelenin drops |
| spellingShingle | T. A. Golomazova N. P. Antonova N. E. Semenova E. P. Shefer S. S. Prokhvatilova Development and Validation of an Analytical Procedure for Determining Convallatoxin in Medicinal Products Containing Cardiac Glycosides of Lily of the Valley Регуляторные исследования и экспертиза лекарственных средств cardiac glycosides convallatoxin high-performance liquid chromatography hplc lily-of-the-valley herb herbal medicinal products zelenin drops |
| title | Development and Validation of an Analytical Procedure for Determining Convallatoxin in Medicinal Products Containing Cardiac Glycosides of Lily of the Valley |
| title_full | Development and Validation of an Analytical Procedure for Determining Convallatoxin in Medicinal Products Containing Cardiac Glycosides of Lily of the Valley |
| title_fullStr | Development and Validation of an Analytical Procedure for Determining Convallatoxin in Medicinal Products Containing Cardiac Glycosides of Lily of the Valley |
| title_full_unstemmed | Development and Validation of an Analytical Procedure for Determining Convallatoxin in Medicinal Products Containing Cardiac Glycosides of Lily of the Valley |
| title_short | Development and Validation of an Analytical Procedure for Determining Convallatoxin in Medicinal Products Containing Cardiac Glycosides of Lily of the Valley |
| title_sort | development and validation of an analytical procedure for determining convallatoxin in medicinal products containing cardiac glycosides of lily of the valley |
| topic | cardiac glycosides convallatoxin high-performance liquid chromatography hplc lily-of-the-valley herb herbal medicinal products zelenin drops |
| url | https://www.vedomostincesmp.ru/jour/article/view/714 |
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