黄杨宁片及原料中环维黄杨星D含量测定的3种HPLC方法评价

Evaluation on Three HPLC Methods on the Determination of Cyclovirobuxium D in Huangyangning Tablets and Raw Materials

关键词:  黄杨宁片  环维黄杨星D  高效液相色谱法  药典

Key words:  Huangyangning tablets  cyclovirobuxium D  HPLC  pharmacopoeia

摘要:

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。

Abstract:

OBJECTIVE To screen out the most reliable and accurate method for Ch.P by comparison on three HPLC methods on the determination of cyclovirobuxium D and evaluation on the method's accuracy, intermediate precision and practicability. METHODS NP-HPLC method with SiO2 column and ELSD detection, NP-HPLC method with NH2 column and end-wavelength detection, and ion-pair RP-HPLC method with C18 column and end-wavelength detection were employed to determine cyclovirobuxium D in huangyangning tablets and raw materials, the method evaluation was given following the chromatographic features, content results, method sensitivities, accuracy and intermediate precision which were compared. RESULTS The raw materials separated by 3 methods could substantially occure 8, 10 and 14 peaks respectively, the recoveries (n=9) were 96.38% (RSD=2.6%), 75.24% (RSD=3.2%) and 97.97% (RSD=1.1%), and the intermediate precision of instruments expressed as RSD (n=3) were 3.9%, 7.1%, 4.0% for tablets and 3.5%, 4.3%, 4.7% for raw materials. CONCLUSION Among 3 methods, in terms of accuracy, intermediate precision and practicability, the ion-pair RP-HPLC method performed best. Therefore it could be adopted as a pharmacopoeia method.