Quality assessment of Chrysanthemum indicum Flower by simultaneous quantification of six major ingredients using a single reference standard combined with HPLC fingerprint analysis

Chrysanthemum indicum Flower is usually consumed as functional food. This paper described an improved total quality assessment method for Chrysanthemum indicum Flower by simultaneous quantitation using a single standard to determine multi-components method combined with high performance liquid chromatography fingerprint analysis. Six main components of Chrysanthemum indicum Flower including two flavonoids and four phenolic acids were simultaneously quantified using linarin as the internal reference standard. The method was fully validated with respect to linearity, precision, accuracy, robustness and stability.The validated method was successfully applied to the analysis of thirty three batches of Chrysanthemum indicum Flower samples. Under the same chromatographic conditions, fingerprint analysis in combination with Similarity analysis and principal component analysis was performed to identify the samples from different regions. In general, an effective assessment using a single standard to determinate multi-components method combined with fingerprint analysis make the reliable qualitation and quantitation analysis of Chrysanthemum indicum Flower available.

Simultaneous Determination of Four Anthraquinones in Polygoni Multiflori Radix with Single Reference Standard by High Performance Liquid Chromatography

Objective: To establish a rapid, accurate and reliable analytical method for the simultaneous determination of four major anthraquinones in Polygoni Multiflori Radix(PMR) using single reference standard.Methods: The four components including emodin-8-O-β-D-(EMG), physcion-8-O-β-D-glucoside, emodin and physcion were separated on an ODS C18 column within 13 min and detected at 280 nm. Emodin was selected as the reference standard, and the response factor for each analyte with respect to emodin were calculated. Robustness were also tested including different columns, equipments, temperatures, detection wavelengths, and other chromatographic conditions which might influence stability of response factors.Results: The method was validated in terms of linearity(r^2> 0.9995), LOQs(0.820–3.05 ng/m L), LODs(0.180–0.920 ng/m L), precision,accuracy(95.8–103.6%, RSD < 2.80%) and stability. A total of 40 batches of PMR were analyzed and the results were found to have no statistically significant differences compared with those obtained using the external standard method.Conclusion: This work provided a single standard to determine multi-components method for quantitation of four anthraquinones in PMR,which could be applied in the quality control of this herbal drug.

骨髓炎颗粒HPLC指纹图谱及一测多评法测定7种成分含量

目的建立骨髓炎颗粒的HPLC指纹图谱及一测多评法(QAMS)测定骨髓炎颗粒中绿原酸、连翘酯苷、芦丁、黄芩素、黄芩苷、汉黄芩苷、党参炔苷等7种主要成分的含量。方法采用Diamonsil-C18色谱柱(150 mm×4.6 mm,4μm),以乙腈-0.1%的磷酸水溶液为流动相,梯度洗脱,流速为1.0 mL·mL^(-1),柱温为30℃,检测波长为280 nm,建立骨髓炎颗粒HPLC指纹图谱与测定绿原酸、连翘酯苷、芦丁、黄芩素、黄芩苷、汉黄芩苷、党参炔苷等7种主要成分含量。结果10批样品共标定了26个共有峰,指认了7个峰,相似度均大于0.995。以黄芩苷为内参物,分别建立绿原酸、芦丁、连翘酯苷、黄芩素、汉黄芩苷、党参炔苷的相对校正因子分别为2.3131、4.1377、2.1300、0.7248、1.9161、8.1718;其校正因子在不同色谱条件下的RSD均小于2%。该6种成分含量用外标法进行测定,与QAMS法比较成分含量结果无明显差异。结论建立的HPLC指纹图谱及7种成分QAMS法,科学合理、简便易行,可用于骨髓炎颗粒中有效成分含量的测定,为深入研究其质量标准奠定基础。

“一测多评”法与外标法测定三黄片中4种黄芩黄酮类成分

目的采用"一测多评"法(QAMS)与外标法(ESM)同步测定三黄片(大黄、盐酸小檗碱及黄芩浸膏)中的4种黄芩黄酮类成分含有量并进行比较,以验证"一测多评"法在三黄片中应用的可行性。方法以黄芩苷为内参物,采用XtimateTMC18(4.6 mm×250 mm,5μm)色谱柱,流动相为甲醇-0.2%磷酸水溶液,梯度洗脱,体积流量为1 mL/min,柱温30℃,检测波长274 nm。结果 2种方法测得的含有量无显著性差异,RSD<5%。结论 "一测多评"法可用于三黄片中4种黄芩黄酮类成分的质量评价。

一测多评法测定小儿咳喘灵颗粒中6种绿原酸类成分的含量

目的:建立小儿咳喘灵颗粒中6种主要活性成分的一测多评含量测定方法。方法:以绿原酸为内标物,采用高效液相色谱方法,建立其与新绿原酸、隐绿原酸、异绿原酸B、异绿原酸A、4,5-O-二咖啡酰奎宁酸5种成分的相对校正因子,并用该校正因子进行计算,实现一测多评;同时采用外标法对6种成分进行含量测定,通过比较两种方法的结果,验证该方法的准确性。结果:建立的校正因子重复性较好,采用校正因子计算的含量值与外标法实测值偏差较好,相对误差<5%。结论:采用一测多评法测定小儿咳喘灵颗粒中6种绿原酸类成分可行。

一测多评法测定小活络丸中9种乌头类生物碱的含量

目的:建立一测多评法同时测定小活络丸中9种乌头类生物碱含量。方法:采用高效液相色谱四级杆飞行时间串联质谱(HPLC-QTOF-MS)法,采用Agilent ZORBAX Extend-C_(18)RRHT(2.1 mm×50 mm,1.8μm)色谱柱;流速为0.21 ml·min^(-1);柱温为30℃;以甲醇为流动相A,以水(含0.1%甲酸和2.5 mmol·L^(-1)醋酸铵溶液)为流动相B,梯度洗脱。以乌头碱为内参物,测定次乌头碱、新乌头碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、苯甲酰新乌头原碱、乌头原碱、次乌头原碱、新乌头原碱对于其的相对校正因子,并对相对校正因子进行重现性考察。利用相对校正因子计算其他8种生物碱成分的含量,同时利用外标法测定这9种成分,比较两种测定方法的差异,验证一测多评法的准确性和可行性。结果:在线性范围内,次乌头碱、新乌头碱、苯甲酰乌头原碱、苯甲酰次乌头碱、苯甲酰新乌头原碱、乌头原碱、次乌头原碱、新乌头原碱对乌头碱的相对校正因于分别为1.736、1.979、1.0471、0.9242、1.2901、1.3078、1.2859、1.0948,建立了QAMS法测定小活络丸中9种生物碱的含量,其测定值与计算值无显著差异。结论:本文方法可用于小活络丸中乌头碱、次乌头碱、新乌头碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、苯甲酰新乌头原碱、乌头原碱、次乌头原碱、新乌头原碱的含量测定。

A feasible,economical,and accurate analytical method for simultaneous determination of six alkaloid markers in Aconiti Lateralis Radix Praeparata from different manufacturing sources and processing ways

Aconiti Lateralis Radix Praeparata(Fuzi) is a commonly used traditional Chinese medicine in clinic for its potency in restoring yang and rescuing from collapse. Aconiti alkaloids, mainly including monoester-diterpenoidaconitines(MDAs) and diester-diterpenoidaconitines(DDAs), are considered to act as both bioactive and toxic constituents. In the present study, a feasible, economical, and accurate HPLC method for simultaneous determination of six alkaloid markers using the Single Standard for Determination of Multi-Components(SSDMC) method was developed and fully validated. Benzoylmesaconine was used as the unique reference standard. This method was proven as accurate(recovery varying between 97.5%-101.8%, RSD < 3%), precise(RSD 0.63%-2.05%), and linear(R > 0.999 9) over the concentration ranges, and subsequently applied to quantitative evaluation of 62 batches of samples, among which 45 batches were from good manufacturing practice(GMP) facilities and 17 batches from the drug market. The contents were then analyzed by principal component analysis(PCA) and homogeneity test. The present study provided valuable information for improving the quality standard of Aconiti Lateralis Radix Praeparata. The developed method also has the potential in analysis of other Aconitum species, such as Aconitum carmichaelii(prepared parent root) and Aconitum kusnezoffii(prepared root).

基于一测多评法的丹参酮提取物质量控制

目的:建立丹参酮提取物中二氢丹参酮I、隐丹参酮、丹参酮I和丹参酮IIA 4种丹参酮类成分的一测多评法,探讨一测多评法在丹参酮提取物质量控制中的应用。方法:采用高效液相色谱法,以丹参酮IIA为内标物,计算二氢丹参酮I、隐丹参酮和丹参酮I相对于丹参酮IIA的相对校正因子和相对保留时间,利用相对校正因子计算丹参酮提取物中4种丹参酮类成分的含量,实现一测多评;同时采用外标法测定4种丹参酮类成分的含量,并比较二者差异,评价一测多评法在丹参酮提取物质量控制应用中的准确性和科学性。结果:二氢丹参酮I、隐丹参酮和丹参酮I相对于丹参酮IIA的相对校正因子分别为1.55、1.12和1.28;各成分的相对校正因子和相对保留时间在不同实验条件下的系统耐用性良好;一测多评法计算结果与外标法测定结果无显著差异。结论:以丹参酮IIA为内标物,建立的丹参酮提取物中4种丹参酮类成分的一测多评方法简便、准确、可靠,可用于丹参酮提取物的多成分质量控制。

光谱法直接测定^(235)U

一、前言光谱分析铀同位素的优点是设备简单,操作方便,比常用的质谱分析经济、快速、无记忆效应,直至目前,在核燃料循环中仍用于测定同位素的丰度。考虑到回收料U_3O_8仅需一般中等精度分析其丰度,故开展了铀同位素光谱分析试验。采用ИСП-51型光谱仪,加工了相板记录和光电记录两用暗合。

一测多评法同时测定白芷配方颗粒中6种成分的含量

目的 建立一测多评法同时测定白芷配方颗粒中6种香豆素类成分的含量。方法 采用UPLC法,色谱柱为Agilent ZORBAX SB-C_(18)(2.1 mm×100 mm,1.8 μm),以乙腈-0.1%乙酸为流动相,梯度洗脱,检测波长为300 nm,流速为0.35 mL·min^(-1),柱温为35℃。以欧前胡素为内参物,建立其与水合氧化前胡素、白当归素、佛手柑内酯、珊瑚菜素、异欧前胡素的相对校正因子,考察其耐用性,计算6种成分含量,并与外标法的含量测定结果比较。结果 在各自线性范围内,水合氧化前胡素、白当归素、佛手柑内酯、珊瑚菜素、异欧前胡素的相对校正因子分别为1.22、1.52、0.79、3.20、1.05;在不同实验条件下相对校正因子耐用性良好,14批白芷配方颗粒的一测多评法与外标法测定结果无显著差异。结论 建立的一测多评法准确可行,可为白芷配方颗粒多指标成分质量评价提供参考。

相对校正因子在中药多指标测定中的应用研究进展

中药标准物质品种和质量的相对滞后,已成为中药标准制定与提高的制约因素,为解决这一问题,不断涌现出新的测定方法。重点介绍与相对校正因子相关的一测多评法、替代对照品法、内标多控法及系统内标法等多指标定量方法;阐述了相对校正因子计算方法相关内容和技术要求,并对其在中药多指标质量控制中的应用情况进行论述。

一测多评法测定黄连须中的5种生物碱

目的采用一测多评法同时测定黄连须中5种生物碱(盐酸小檗碱、盐酸药根碱、盐酸表小檗碱、盐酸黄连碱和盐酸巴马汀)的含量。方法以盐酸小檗碱为内参物,采用HPLC法测定其与盐酸药根碱、盐酸表小檗碱、盐酸黄连碱、盐酸巴马汀的相对校正因子,利用该相对校正因子计算其他4种生物碱的含量;同时利用外标法测定5种生物碱的含量,比较两种测定方法的差异,验证一测多评法的可行性和准确性。结果在线性范围内,盐酸小檗碱与盐酸药根碱、盐酸表小檗碱、盐酸黄连碱、盐酸巴马汀的相对校正因子分别为1.128、1.008、1.070、1.025,在不同实验条件下,相对校正因子的重复性良好,5种生物碱成分含量的计算值与实测值间无显著性差异。结论一测多评法同时测定黄连须中5种生物碱的含量是可行的、准确的。