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

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.

Development of a new ferulic acid certified reference material for use in clinical chemistry and pharmaceutical analysis

This study compares the results of three certified methods,namely differential scanning calorimetry(DSC),the mass balance(MB) method and coulometric titrimetry(CT),in the purity assessment of ferulic acid certified reference material(CRM).Purity and expanded uncertainty as determined by the three methods were respectively 99.81%,0.16%;99.79%,0.16%;and 99.81%,0.26%with,in all cases,a coverage factor(k) of 2(P ? 95%).The purity results are consistent indicating that the combination of DSC,the MB method and CT provides a confident assessment of the purity of suitable CRMs like ferulic acid.

Theoretical and experimental assessment of a novel method to establish the complete measurement range of the calorimeter and its limit of detection and quantification

For determining the accuracy of a calorimeter over the instrument’s entire measuring range,a novel method has been established.For this new approach,(a)benzoic acid(C_(6)H_(5)CO_(2)H) as a certified reference material(CRM),(b)SiO_(2) and(c)a mixture of CRM benzoic acid and SiO_(2) have been used.To illustrate the essential difference between 1)the novel analytical method for control of the entire measurement range and 2)the calorimeter calibration,both applications of benzoic acid(BA)have been demonstrated.An experimental result showed that BA was successfully used to check the whole calorimeter measurement range.The results also showed that the same new method was successfully applied to determine the limit of detection and quantification.A new instrument testing process and a new measurement technique have thus been established.In this way,the cost of using CRM to control the accuracy of measuring the entire measuring range of the calorimeter,as shown in this paper,is minimized.The requirements of the ISO/IEC 17025:2017 standard are satisfied.ISO/IEC 17025:2017,together with ISO 9001:2015(quality management systems),ISO 14001:2015(relate to environmental protection)and ISO45001:2018(occupational safety),constitute an integrated quality system by which a testing laboratory may also accredit.

一种感官检验用玉米不完善粒标准样品的制备

Maize unsound kernel content is one of the limited items in maize trade, and generally determined by sensory detection. A certified reference material(CRM) for visual inspection of maize unsound kernels was developed according to a national standard of China, GB 1353-2018, and five items, such as insect-damaged kernels, spotted kernels, broken kernels, sprouted kernels and moldy kernels, were included. Unsound maize kernels were collected from fields or prepared in a laboratory, then screened, and ten kernels demonstrating varying levels of unsoundness or damage for each item were embedded in epoxy resin. The CRM showed excellent homogeneity and stability, which was stable for 14 days at the temperature from-20℃ to 45℃ and for at least 18 months at room temperature out of direct sunlight and strong light. Co-laboratory confirmation showed the CRM conformed to the morphological characteristics described in GB 1353-2018. The research filled the gap of unsound maize kernel CRM in maize detection.