HPLC-DAD法同时测定中药苦参中七种生物碱成分的含量

目的:建立HPLC-DAD法同时测定中药苦参中氧化槐醇碱、氧化苦参碱、槐定碱、氧化槐果碱、槐醇、苦参碱及槐果碱七种生物碱的含量。方法:Agilent Zorbax C_(18)色谱柱(150 mm×4.6 mm,5μm),流动相为10 mmol·L^(-1)醋酸铵水溶液(0.05%氨水,p H=9.0)(A)-20 mmol·L^(-1)醋酸铵的甲醇-乙腈(1∶2)混合溶液(B),梯度洗脱,流速:1.0 ml·min^(-1),检测波长:220 nm,柱温:30℃。结果:氧化槐醇碱、氧化苦参碱、槐定碱、氧化槐果碱、槐醇、苦参碱及槐果碱的质量浓度分别在0.093~1.860μg(r=0.999 6)、0.530~10.600μg(r=0.999 7)、0.062~1.240μg(r=0.999 8)、0.281~5.620μg(r=0.999 9)、0.026~0.520μg(r=0.999 8)、0.036~0.720μg(r=0.999 7)及0.032~0.640μg(r=0.999 6)内与峰面积呈良好的线性关系。氧化槐醇碱、氧化苦参碱、槐定碱、氧化槐果碱、槐醇、苦参碱及槐果碱的平均加样回收率分别为97.5%、98.2%、99.0%、99.4%、99.2%、98.2%和98.7%,RSD分别为1.18%、0.92%、1.43%、1.04%、0.81%、0.43%和0.88%(n=6)。结论:该方法简便、准确、重复性好,可用于苦参药材多成分的质量控制研究。

HPLC-DAD法同时测定罗布麻中4种黄酮类成分含量

目的:建立HPLC-DAD法对罗布麻药材中金丝桃苷、芦丁、槲皮素、异槲皮苷4种黄酮类成分含量进行测定。方法:色谱柱:Shiseido C18(3.0μm,3.0mm×100mm);流动相:乙腈∶甲醇(10∶1),梯度洗脱,流速为0.6mL·min^(-1);柱温为30℃;波长为360nm。结果:金丝桃苷、芦丁、槲皮素与异槲皮苷回归方程分别为:Y=15.58X+1.173,r=0.999;Y=11.73X-0.388,r=0.999;Y=12.52X-0.3.222,r=0.999;Y=18.42X+1.481,r=0.999。线性范围分别为:0.8775~87.75μg·mL^(-1),0.3083~30.83μg·mL^(-1),0.249 7~24.97μg·mL^(-1),0.9019~90.21μg·mL^(-1);平均RSD分别为0.26%、0.53%、0.92%、0.19%。结论:HPLC-DAD法同时测定罗布麻黄酮类成分含量,具有较高准确性、快捷性、简便性、重复性。

Optimization of extraction and determination of emodin from Polygonum cuspidatum Sieb. et Zucc. products by HPLC-DAD

A uniform experimental design procedure was used to investigate the effects of some operating parameters on the extraction of emodin from Polygonum cuspidatum Sieb. et Zucc. products. Variables tested were volume ratio of material to solvent, size of material, extraction time and temperature and composition of extraction solvent （mixtures of acetone-water）. Each variable was tested at seven levels; 7 experiments were performed in random order. Analyses of the extracts were performed by high-performance liquid chromatography with diode array detection（HPLC-DAD）. Analytical responses were processed by using a forward regression analysis, in order to find polynomial function describing the relationship between variables and responses. For all the analytes the experimental conditions for providing the highest extraction yield inside the experimental domain considered were found. Finally, a simple, rapid and accurate analytical method was developed for the determination of emodin by high performance liquid chromatography. The separation is achieved within 25 rain on an ODS column using methanol and water as gradient mobiles. Emodin can be quantified by using external standard method detecting at 436 nm. Good linearity is obtained with correlation coefficient exceeding 0.9986 and the detection limit and the quantification limit are 1.53 and 3.23 mg/L respectively. This method shows good reproducibility for the quantification of the emodin with intra-day and inter-day relative standard deviation less than 2.3% and 5.6% respectively. Under optimized extraction conditions, the recovery of the standard is 96.5%. The validated method is successfully applied to quantify the emodin in seven Polygonum cuspidatum sieb. Et zucc. products, which provided an idea for the pre-treatment of determination of active compounds in traditional Chinese medicines.

小儿肺炎口服液的质量标准研究

目的：建立小儿肺炎口服液主要成分的含量测定方法，为该制剂的质量控制提供参考。方法：采用高效液相色谱．二极管阵列检测器（HPLC—DAD）法分别对小儿肺炎口服液中的主要成分盐酸麻黄碱、盐酸伪麻黄碱、盐酸小檗碱、黄芩苷、大黄素、大黄酚、紫菀酮进行定量分析。结果：所测定的主要成分在其最大吸收波长下均达到基线分离，线性范围较宽，盐酸麻黄碱在0．1013—0．5065mg／mL（r=0．9998）、盐酸伪麻黄碱在0．1040～0．5200mg／mL（r=0，9999）、盐酸小檗碱在O．1852—0．9260m/mL（r=0．9999）、黄芩苷在1．0500～5．2500mg／mL（r=0．9999）、大黄素在0．0028～0．0142mg／mL（r=0．9997）、大黄酚在0．0023—0．0114mg／mL（r=0．9996）、紫菀酮在0．0392—0．3136mg／mL（r=0．9996）范围内与峰面积线性关系良好，平均回收率在95．0％以上。结论：HPLC—DAD法测定小儿肺炎口服液主要成分含量方法简便、准确、重复性好，可用于小儿肺炎口服液的质量控制。