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目的通过比较环维黄杨星D的3种高效液相色谱测定方法,对方法准确性、中间精密度和实用性作出评价,以筛选出适合作为药典标准的方法。方法分别采用SiO2柱正相高效液相色谱ELSD检测法、NH2柱正相高效液相色谱末端检测法、C18柱反相离子对高效液相色谱末端检测法分别对黄杨宁片及原料进行测定,比较其色谱行为、含量、灵敏度、中间精密度和准确性,并给出评价。结果3种方法使原料分离出的最多峰数分别为8,10,14个;回收率(n=9)分别为96.38%(RSD=2.6%)、75.24%(RSD=3.2%)、97.97%(RSD=1.1%);不同仪器上的含量中间精密度RSD(n=3)片剂分别为3.9%,7.1%,4.0%,原料分别为3.5%,4.3%,4.7%。结论3种方法中,综合准确性、中间精密度、实用性等方面因素,C18柱反相离子对色谱末端检测法为最佳,适合作为药典方法。
Objective To evaluate the accuracy, intermediate precision and practicality of the method by comparing three HPLC methods for measuring Cyclovirobuxine D, so as to screen out suitable methods for pharmacopoeia standards. Methods Positive-phase HPLC chromatographic (ELSD) detection was performed on SiO2 column, normal-phase HPLC end-point detection on NH2 column and reversed-phase ion-pair high-performance liquid chromatography (HPLC) end detection on C18 column. The chromatographic behavior, content, sensitivity, intermediate precision, and accuracy were compared and evaluated. Results The maximum number of peaks isolated from the three methods was 8, 10, and 14 respectively. The recoveries (n=9) were 96.38% (RSD=2.6%), 75.24% (RSD=3.2%), and 97.97%, respectively. (RSD = 1.1%); the intermediate precision RSD (n = 3) tablets on different instruments were 3.9%, 7.1%, and 4.0%, respectively, and the raw materials were 3.5%, 4.3%, and 4.7%, respectively. Conclusion Among the three methods, the accuracy, intermediate precision, practicality and other factors were the best. The C18 column reverse phase ion pair chromatography end detection method was the best and suitable as a pharmacopoeia method.