The emerging development of Extractive Reference Substance (ERS) is a methodology that meets the needs for quality control for Chinese Herbal Medicines (CHM) and respects the holistic viewpoint of Traditional Chinese ...The emerging development of Extractive Reference Substance (ERS) is a methodology that meets the needs for quality control for Chinese Herbal Medicines (CHM) and respects the holistic viewpoint of Traditional Chinese Medicine (TCM) and its clinical use of multiple ingredients with synergistic effects. The convention of using just a selected few Chemical Reference Substances (CRS) cannot adequately assess the quality of intact CHM. A validated chemical spectrum of an ERS provides the global characteristics in order to more specifically identify and assess targeted CHM. This paper describes the fundamental concepts, potential significance, and basic criteria of ERS, along with methods of preparation and calibration. Given the diversity of CHM, the various problems that will occur in establishing the proper process of ERS will need to be solved in a step by step manner. The ERSs of Ziziphi spinosae semen and ERS of Fritillaria thunbergii bulbus are given as examples of the development of ERS and demonstrate why we are optimistic about the utility of this approach.展开更多
An HPLC method for quantitative determination of adrenaline hydrochloride injection and noradrenaline bitartrate injection was established and validated with a substitute for the reference substance.Phenylephrine hydr...An HPLC method for quantitative determination of adrenaline hydrochloride injection and noradrenaline bitartrate injection was established and validated with a substitute for the reference substance.Phenylephrine hydrochloride was selected as the substitute for the reference substance of adrenaline and noradrenaline bitartrate.The correction factor of phenylephrine hydrochloride with respect to the reference substance of adrenaline and noradrenaline bitartrate was determined under defined conditions.Adrenaline hydrochloride injection and noradrenaline bitartrate injection were quantified by assaying phenylephrine hydrochloride and a correct factor.The results indicate that the HPLC method with the substitute for reference substance was reliable and feasible for quantitative determination of drugs.展开更多
In this article, the block scheme and metrological characteristics of the State primary standard of the mass (molar) fraction and mass (molar) concentration of the component in the liquid and solid substances and mate...In this article, the block scheme and metrological characteristics of the State primary standard of the mass (molar) fraction and mass (molar) concentration of the component in the liquid and solid substances and materials based on coulometric titration GET 176-2010 are given. Primary reference materials certified by coulometric titration in the Ural Scientific and Research Institute for Metrology include eight certified reference materials (CRMs) of pure solid substances (mostly salts of sodium or potassium) and one hydrochloric acid solution CRM. The metrological characteristics of these reference materials and the scheme of their application in titrimetric analysis are shown. The expanded uncertainty of the certified value (mass fraction for the solid substances or molar concentration for the solution) is in the range from 0.018% to 0.05%. Information about two primary reference materials of high purity iron and lead nitrate certified by controlled-potential coulometry with expanded uncertainty from 0.04% to 0.07% is also given.展开更多
目的建立基于制剂中多种内参物的一测多评法(quantitative analysis of multi-components by single-marker,QAMS)以测定双香消食化积胶囊中5种成分的含量。方法色谱柱为Agilent Eclipse plus C18(250 mm×4.6 mm,5μm),流动相为乙...目的建立基于制剂中多种内参物的一测多评法(quantitative analysis of multi-components by single-marker,QAMS)以测定双香消食化积胶囊中5种成分的含量。方法色谱柱为Agilent Eclipse plus C18(250 mm×4.6 mm,5μm),流动相为乙腈-体积分数0.05%磷酸溶液(梯度洗脱),流速为1.0 mL·min^(−1),柱温为30℃,检测波长为283 nm。分别以芸香柚皮苷、柚皮苷、橙皮苷、和厚朴酚、厚朴酚为内参物,采用QAMS建立另外4个待测成分与内参物的相对校正因子,计算7批双香消食化积胶囊样品中5个成分的含量,并与用外标法(external standard method,ESM)测定的结果进行比较。结果用QAMS测得7批双香消食化积胶囊样品中芸香柚皮苷、柚皮苷、橙皮苷、和厚朴酚、厚朴酚的含量分别为1.353~1.845、5.865~6.417、8.150~9.539、1.088~1.241、3.321~4.455 mg·g^(−1),ESM测定结果分别为1.345~1.840、5.882~6.435、8.167~9.563、1.093~1.247、3.312~4.433 mg·g^(−1),用2种方法得到的结果的差异百分比≤1.00%,并通过统计比较ESM和QAMS测出的2组数据Pearson相关系数相似度较高,差异无统计学意义(P>0.05)。结论建立了基于制剂中多种内参物同时测定双香消食化积胶囊中5种成分含量的QAMS。该方法与ESM所得结果无明显差异,可用于双香消食化积胶囊的质量控制。展开更多
Objective:In order to evaluate the reliability and feasibility of pueraria reference extractive substance(RES)used in biological sample,the pharmacokinetics of 3–hydroxy puerarin(3-HP),puerarin,3–methoxy puerarin(3-...Objective:In order to evaluate the reliability and feasibility of pueraria reference extractive substance(RES)used in biological sample,the pharmacokinetics of 3–hydroxy puerarin(3-HP),puerarin,3–methoxy puerarin(3-MP),and daidzein-8-C-apiosyl-(1-6)-glucoside(DAG)in beagle plasma following oral administration of Yufeng Ningxin Tablet were quantitated.Methods:A reliable and sensitive high-performance liquid chromatography-tandem triple quadrupole mass spectrometry(HPLC-QQQ-MS/MS)method developed with chromatographic separation was operated on a Merck C18 column,and acetonitrile-5 mmol/L ammonium was used as mobile phase in gradient elution.The plasma samples were deproteinized by acetone,detected by triple quadrupole mass spectrometry with an electrospray ionization interface,and quantified using selected ion monitoring mode.The pharmacokinetic parameters were calculated by Winnonlin 4.1.Results:The calibration curves of the reference extractive substance and standard substance methods were linear over the ranges 0.0417–11.3309μg/m L and 0.0394–10.0000μg/m L.The intra-day and interday precision of the two methods at three concentrations were less than 13.63%,and the average recoveries of 3-HP,puerarin,3-MP,and DAG were more than 70.67%.The RSD of the mean plasma concentrations of the analytes calculated by the two methods was less than 5%,and cos(?)==1.000.Among the analytes,puerarin showed the highest blood concentration[(940±185)ng/m L]and the longest retention time[(5±1)h]in the dog’s bodies.Conclusion:Pueraria reference extractive substance can be seen as an alternative to the standard substance to overcome the scarcity of standard substance for the analysis of biological samples.展开更多
文摘The emerging development of Extractive Reference Substance (ERS) is a methodology that meets the needs for quality control for Chinese Herbal Medicines (CHM) and respects the holistic viewpoint of Traditional Chinese Medicine (TCM) and its clinical use of multiple ingredients with synergistic effects. The convention of using just a selected few Chemical Reference Substances (CRS) cannot adequately assess the quality of intact CHM. A validated chemical spectrum of an ERS provides the global characteristics in order to more specifically identify and assess targeted CHM. This paper describes the fundamental concepts, potential significance, and basic criteria of ERS, along with methods of preparation and calibration. Given the diversity of CHM, the various problems that will occur in establishing the proper process of ERS will need to be solved in a step by step manner. The ERSs of Ziziphi spinosae semen and ERS of Fritillaria thunbergii bulbus are given as examples of the development of ERS and demonstrate why we are optimistic about the utility of this approach.
文摘An HPLC method for quantitative determination of adrenaline hydrochloride injection and noradrenaline bitartrate injection was established and validated with a substitute for the reference substance.Phenylephrine hydrochloride was selected as the substitute for the reference substance of adrenaline and noradrenaline bitartrate.The correction factor of phenylephrine hydrochloride with respect to the reference substance of adrenaline and noradrenaline bitartrate was determined under defined conditions.Adrenaline hydrochloride injection and noradrenaline bitartrate injection were quantified by assaying phenylephrine hydrochloride and a correct factor.The results indicate that the HPLC method with the substitute for reference substance was reliable and feasible for quantitative determination of drugs.
文摘In this article, the block scheme and metrological characteristics of the State primary standard of the mass (molar) fraction and mass (molar) concentration of the component in the liquid and solid substances and materials based on coulometric titration GET 176-2010 are given. Primary reference materials certified by coulometric titration in the Ural Scientific and Research Institute for Metrology include eight certified reference materials (CRMs) of pure solid substances (mostly salts of sodium or potassium) and one hydrochloric acid solution CRM. The metrological characteristics of these reference materials and the scheme of their application in titrimetric analysis are shown. The expanded uncertainty of the certified value (mass fraction for the solid substances or molar concentration for the solution) is in the range from 0.018% to 0.05%. Information about two primary reference materials of high purity iron and lead nitrate certified by controlled-potential coulometry with expanded uncertainty from 0.04% to 0.07% is also given.
文摘目的建立基于制剂中多种内参物的一测多评法(quantitative analysis of multi-components by single-marker,QAMS)以测定双香消食化积胶囊中5种成分的含量。方法色谱柱为Agilent Eclipse plus C18(250 mm×4.6 mm,5μm),流动相为乙腈-体积分数0.05%磷酸溶液(梯度洗脱),流速为1.0 mL·min^(−1),柱温为30℃,检测波长为283 nm。分别以芸香柚皮苷、柚皮苷、橙皮苷、和厚朴酚、厚朴酚为内参物,采用QAMS建立另外4个待测成分与内参物的相对校正因子,计算7批双香消食化积胶囊样品中5个成分的含量,并与用外标法(external standard method,ESM)测定的结果进行比较。结果用QAMS测得7批双香消食化积胶囊样品中芸香柚皮苷、柚皮苷、橙皮苷、和厚朴酚、厚朴酚的含量分别为1.353~1.845、5.865~6.417、8.150~9.539、1.088~1.241、3.321~4.455 mg·g^(−1),ESM测定结果分别为1.345~1.840、5.882~6.435、8.167~9.563、1.093~1.247、3.312~4.433 mg·g^(−1),用2种方法得到的结果的差异百分比≤1.00%,并通过统计比较ESM和QAMS测出的2组数据Pearson相关系数相似度较高,差异无统计学意义(P>0.05)。结论建立了基于制剂中多种内参物同时测定双香消食化积胶囊中5种成分含量的QAMS。该方法与ESM所得结果无明显差异,可用于双香消食化积胶囊的质量控制。
基金financial support from the Major or Scientific and Technological Special Project for“Significant New Drug Creation”(No.2014ZX0930437)the support of Conservation Propagation and Quality Standard of Characteristic Advantage of Chinese Herbal Medicine(No.2015BAI05B03)+1 种基金Bijie City Achievement Transformation Project(Bi Ke Cheng Zi[2014]No.8)Bijie City Social Development Project(Bi Kehe Zi[2015]No.41).
文摘Objective:In order to evaluate the reliability and feasibility of pueraria reference extractive substance(RES)used in biological sample,the pharmacokinetics of 3–hydroxy puerarin(3-HP),puerarin,3–methoxy puerarin(3-MP),and daidzein-8-C-apiosyl-(1-6)-glucoside(DAG)in beagle plasma following oral administration of Yufeng Ningxin Tablet were quantitated.Methods:A reliable and sensitive high-performance liquid chromatography-tandem triple quadrupole mass spectrometry(HPLC-QQQ-MS/MS)method developed with chromatographic separation was operated on a Merck C18 column,and acetonitrile-5 mmol/L ammonium was used as mobile phase in gradient elution.The plasma samples were deproteinized by acetone,detected by triple quadrupole mass spectrometry with an electrospray ionization interface,and quantified using selected ion monitoring mode.The pharmacokinetic parameters were calculated by Winnonlin 4.1.Results:The calibration curves of the reference extractive substance and standard substance methods were linear over the ranges 0.0417–11.3309μg/m L and 0.0394–10.0000μg/m L.The intra-day and interday precision of the two methods at three concentrations were less than 13.63%,and the average recoveries of 3-HP,puerarin,3-MP,and DAG were more than 70.67%.The RSD of the mean plasma concentrations of the analytes calculated by the two methods was less than 5%,and cos(?)==1.000.Among the analytes,puerarin showed the highest blood concentration[(940±185)ng/m L]and the longest retention time[(5±1)h]in the dog’s bodies.Conclusion:Pueraria reference extractive substance can be seen as an alternative to the standard substance to overcome the scarcity of standard substance for the analysis of biological samples.
