HPLC法同时测定胆木及其制剂中酚酸和生物碱类成分  

Simultaneous determination of phenolic acid and three alkaloids in Nauclea officinalis and its preparations by HPLC

作　　者：王静静[1,2] 蒋俊[3] 朱粉霞[2] 李秀峰 贾晓斌[1,2] 

机构地区：[1]江苏大学药学院,江苏镇江212013 [2]江苏省中医药研究院国家中医药管理局中药口服释药系统重点研究室,江苏南京210028 [3]镇江出入境检验检疫局,国家食品添加剂及调味剂检测重点实验室,江苏镇江212003 [4]海南制药厂有限公司黎药工程中心,海南五指山572200

出　　处：《中成药》2012年第12期2326-2330,共5页Chinese Traditional Patent Medicine

基　　金：国家自然科学基金资助项目(81203001)

摘　　要：目的建立胆木药材及其制剂中原儿茶酸,短小舌根草苷,3-表短小舌根草苷,异长春花苷内酰胺的测定方法。方法采用HPLC法,X-SELECT CSHTMC18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.05%甲酸水,梯度洗脱;检测波长258 nm(原儿茶酸),243 nm(短小舌根草苷、3-表短小舌根草苷),226 nm(异长春花苷内酰胺);体积流量1 mL/min;柱温30℃。结果原儿茶酸、短小舌根草苷、3-表短小舌根草苷和异长春花苷内酰胺分别在0.966～154.56μg/mL、0.944～151.04μg/mL、0.954～152.64μg/mL和0.916～146.56μg/mL内具有良好的线性关系(R2≥0.999 8);4种成分在胆木药材中的平均加样回收率分别为98.2%、101.3%、97.4%和99.2%,RSD≤3.62%。在胆木注射液中的平均加样回收率为99.7%,103.0%,98.9%,100.7%,RSD≤2.44%。结论本法操作简便,结果可靠,重现性好,可作为胆木药材及其制剂质量控制的方法。AIM To develop a method for simultaneously determining protocatechuic acid,pumiloside,3-epipumiloside and strictosamide in Nauclea officinalis and its preparation—Danmu Injection.METHODS Chromatography was performed on an X-SELECT CSHTM C18 column（250 mm×4.6 mm,5 μm） with the mobile phase of acetonitrile and water containing 0.05% formic acid.The detection wavelengths were set at 258 nm for protocatechuic acid,243 nm for pumiloside and 3-epi-pumiloside,226 nm for strictosamide.The flow rate was 1 mL/min and column temperature was maintained at 30 ℃.RESULTS The correlation coefficients between concentrations and chromatographic peak areas of protocatechuic acid,pumiloside,3-epipumiloside and strictosamide were over 0.999 0 in the ranges of 0.966-154.56 μg/mL,0.944-151.04 μg/mL,0.954-152.64 μg/mL and 0.916-146.56 μg/mL,respectively.The average recoveries of the four compounds of Nauclea officinalis were 98.2%,101.3%,97.4% and 99.2%,respectively with RSD≤3.62%.The average recoveries of the four compounds of Danmu Injection were 99.7%,103.0%,98.9% and 100.7%,respectively with RSD≤2.44%.CONCLUSION The developed HPLC method is simple,accurate and has good reproducibility in separation,which is available for the quality control of Nauclea officinalis and Danmu Injection.

关 键 词：胆木 胆木注射液 酚酸 生物碱 质量控制 高效液相色谱法 

分 类 号：R927.2[医药卫生—药学]