Preparation and Certification of a New Salvianolic Acid A Reference Material for Food and Drug Research

doi:10.1007/s13659-020-00236-2

Natural Products and Bioprospecting ›› 2020, Vol. 10 ›› Issue (2): 67-76.DOI: 10.1007/s13659-020-00236-2

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Preparation and Certification of a New Salvianolic Acid A Reference Material for Food and Drug Research

Dezhi Yang¹, Bin Su², Yancai Bi², Li Zhang¹, Baoxi Zhang¹, Junke Song³, Yang Lu¹, Guanhua Du³

1 Beijing City Key Laboratory of Polymorphic Drugs, Center of Pharmaceutical Polymorphs, Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, Beijing 100050, People's Republic of China;
2 Soteria Pharmaceutical Co., Ltd., Laiwu 271100, People's Republic of China;
3 Beijing City Key Laboratory of Drug Target and Screening Research, National Center for Pharmaceutical Screening, Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, Beijing 100050, People's Republic of China

Received:2020-01-23 Revised:2020-02-19 Online:2020-05-06 Published:2020-04-24
Contact: Yang Lu, Guanhua Du
Supported by:
The authors acknowledge National Key R&D Program of China (Grant No. 2016YFC1000900), The Drug Innovation Major Project (Grant No. 2018ZX09711001-001-015) should be substituted by Drug Innovation Major Project (Grant No. 2018ZX09711001-003-022) and CAMS Innovation Fund for Medical Sciences (Grant No. 2016-I2M-3-007) for financing this work.

Preparation and Certification of a New Salvianolic Acid A Reference Material for Food and Drug Research

Dezhi Yang¹, Bin Su², Yancai Bi², Li Zhang¹, Baoxi Zhang¹, Junke Song³, Yang Lu¹, Guanhua Du³

1 Beijing City Key Laboratory of Polymorphic Drugs, Center of Pharmaceutical Polymorphs, Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, Beijing 100050, People's Republic of China;
2 Soteria Pharmaceutical Co., Ltd., Laiwu 271100, People's Republic of China;
3 Beijing City Key Laboratory of Drug Target and Screening Research, National Center for Pharmaceutical Screening, Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, Beijing 100050, People's Republic of China

通讯作者: Yang Lu, Guanhua Du
基金资助:
The authors acknowledge National Key R&D Program of China (Grant No. 2016YFC1000900), The Drug Innovation Major Project (Grant No. 2018ZX09711001-001-015) should be substituted by Drug Innovation Major Project (Grant No. 2018ZX09711001-003-022) and CAMS Innovation Fund for Medical Sciences (Grant No. 2016-I2M-3-007) for financing this work.

Abstract

Abstract: Salvianolic acid A (Sal A), a water-soluble ingredient in Danshen, has various biological activities. Sal A and its impurities have similar physical and chemical properties, as well as strong reducibility; therefore, they are difficult to prepare and purify. In this study, high-purity Sal A was obtained by purification of sephadex chromatography and preparative chromatography. Furthermore, HPLC-DAD tandem ECD and HPLC-DAD tandem MS methods were used for non-volatile organic impurity analysis, ICP-MS method was used for non-volatile inorganic impurities and mass balance method and quantitative nuclear magnetic resonance were employed to certify the product. The structures of Sal A and its relative impurities were validated by nuclear magnetic resonance spectroscopy and mass spectrometry, and their contents were quantified as well. Following the principles of ISO Guides 34:2009 and 35:2005, a Sal A reference material was certified, covering homogeneity studies, stability studies, characterization, and uncertainty estimations.

Key words: Certified reference material, Salvianolic acid A, Mass balance method, qNMR, High resolution mass spectrum

摘要： Salvianolic acid A (Sal A), a water-soluble ingredient in Danshen, has various biological activities. Sal A and its impurities have similar physical and chemical properties, as well as strong reducibility; therefore, they are difficult to prepare and purify. In this study, high-purity Sal A was obtained by purification of sephadex chromatography and preparative chromatography. Furthermore, HPLC-DAD tandem ECD and HPLC-DAD tandem MS methods were used for non-volatile organic impurity analysis, ICP-MS method was used for non-volatile inorganic impurities and mass balance method and quantitative nuclear magnetic resonance were employed to certify the product. The structures of Sal A and its relative impurities were validated by nuclear magnetic resonance spectroscopy and mass spectrometry, and their contents were quantified as well. Following the principles of ISO Guides 34:2009 and 35:2005, a Sal A reference material was certified, covering homogeneity studies, stability studies, characterization, and uncertainty estimations.

关键词: Certified reference material, Salvianolic acid A, Mass balance method, qNMR, High resolution mass spectrum

Dezhi Yang, Bin Su, Yancai Bi, Li Zhang, Baoxi Zhang, Junke Song, Yang Lu, Guanhua Du. Preparation and Certification of a New Salvianolic Acid A Reference Material for Food and Drug Research[J]. Natural Products and Bioprospecting, 2020, 10(2): 67-76.

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Preparation and Certification of a New Salvianolic Acid A Reference Material for Food and Drug Research

Preparation and Certification of a New Salvianolic Acid A Reference Material for Food and Drug Research

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