Dataset Information

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

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.

SUBMITTER: Yang D

PROVIDER: S-EPMC7176770 | biostudies-literature | 2020 Apr

REPOSITORIES: biostudies-literature

ACCESS DATA

Publications

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

Yang Dezhi D Su Bin B Bi Yancai Y Zhang Li L Zhang Baoxi B Song Junke J Lu Yang Y Du Guanhua G

Natural products and bioprospecting 20200418 2

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, IC ...[more]

PMID: 32306209

Similar Datasets

Project description:Validation of analytical methods for measurements of microplastics (MP) is severely hampered because of a general lack of reference materials, RM. There is a great need to develop such reference materials. This study presents a concept of three-component kit with immobilised MP in solid NaCl, a surfactant and clean water that can be applied for the production of many types of MP RMs. As proof of concept, an RM for polyethylene terephthalate (PET) particles in water was prepared and evaluated for its homogeneity. The particles ranged from 30 μm (Feretmin) to about 200 μm adapted by wet sieving. A specific number of PET particles were immobilized in about 0.29 g of solid NaCl by freeze-drying 1 mL of a NaCl suspension. By using manual and automated counting, twenty reconstituted 1-L water samples were evaluated for homogeneity with respect to number of PET particles from 30 μm to > 200 μm/L of water. The number of particles was 730 ± 120 (mean ± one standard deviation (SD); n = 10) and 865 ± 155 particles (n = 10) obtained by optical microscopy in two independent laboratories. This corresponded to relative SDs of 16.4 and 17.9% and a mean of 797 ± 151 particles (18.9% RSD, for n = 20). Homogeneity studies of the NaCl carrier without reconstitution resulted in 794 ± 60 particles (7.5% RSD). The homogeneity of PET in the salt carrier was also evaluated directly with respect to mass of PET per vial using an ultra-micro balance. An average mass of 293 ± 41 μg of PET was obtained (14, % RSD for n = 14). Micrographs were recorded to demonstrate the absence of major sources of contamination of the RM components. Information about the particle size distribution and particle shapes was obtained by laser diffraction (LD) and dynamic image analysis (DIA). In addition, the identity of the PET polymer was confirmed by Raman and FT-IR spectroscopy. The RM was developed for a large-scale inter-laboratory comparison of PET particles in water (ILC). Based on the homogeneity results, the material was found to be sufficiently homogeneous to be of meaningful use in the ILC. In a 3-day process, more than 500 samples of PET particles in the NaCl carrier were prepared with good potential for further upscaling with respect to the number of vials or with other kinds of polymers. The stability of PET was not evaluated but it was deemed to be stable for the duration of the ILC.

Project description:Well-characterized amphibole asbestos mineral samples are required for use as analytical standards and in future research projects. Currently, the National Institute for Standards and Technology Standard Reference Material samples of asbestos are listed as 'Discontinued'. The National Institute for Occupational Safety and Health (NIOSH) has a goal under the Asbestos Roadmap of locating and characterizing research materials for future use. Where an initial characterization analysis determines that a collected material is appropriate for use as a research material in terms of composition and asbestiform habit, sufficient amounts of the material will be collected to make it publicly available. An abandoned mine near Lone Pine, California, contains a vein of tremolite asbestos, which was the probable source of a reference material that has been available for the past 17 years from the Health and Safety Laboratory (HSL) in the UK. Newly collected fibrous vein material from this mine was analyzed at Research Triangle Institute (RTI International) with some additional analysis by the US Geological Survey's Denver Microbeam Laboratory. The analysis at RTI International included: (i) polarized light microscopy (PLM) with a determination of principal optical properties; (ii) X-ray diffraction; (iii) transmission electron microscopy, including energy dispersive X-ray spectroscopy and selected-area electron diffraction; and (iv) spindle stage analysis using PLM to determine whether individual fibers and bundles of the samples were polycrystalline or single-crystal cleavage fragments. The overall findings of the study indicated that the material is tremolite asbestos with characteristics substantially similar to the earlier distributed HSL reference material. A larger quantity of material was prepared by sorting, acid-washing and mixing for sub-division into vials of ~10g each. These vials have been transferred from NIOSH to RTI International, from where they can be obtained on request.

Dataset Information

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

Publications

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

Similar Datasets

OmicsDI is part of the ELIXIR infrastructure

Tweets