变换波长HPLC法同时测定黄连上清丸中12种成分的含量  

Determination of 12 compounds in Huanglian Shangqing pills by HPLC combined with wavelength switching method

作　　者：许苗苗 王云霞 王舒懿 张鑫 谢锦艳 

机构地区：[1]西安市食品药品检验所,西安710054

出　　处：《中南药学》2016年第8期851-854,共4页Central South Pharmacy

摘　　要：目的建立高效液相色谱波长切换法测定黄连上清丸中12种成分含量的方法。方法采用Welch-Ultimate-C_(18)色谱柱(4.6 mm×250 mm,5μm);以乙腈-0.3%磷酸溶液为流动相;柱温30℃;流速1 m L·min^(-1);切换波长检测。结果在HPLC法中,黄柏碱、甘草苷、黄芩苷、小檗碱、黄芩素、芦荟大黄素、大黄酸、欧前胡素、大黄素、异欧前胡素、大黄酚、大黄素甲醚的线性范围分别是:248~1736 ng(r=0.9996)、82.94~580.58 ng(r=1.0000)、68.54~685.4 ng(r=0.9999)、33.8~236.6 ng(r=0.9996)、149.6~1047.2 ng(r=0.9999)、31.54~220.78 ng(r=1.0000)、27.74~267.4 ng(r=0.9998)、7.68~53.76 ng(r=0.9999)、32.84~229.88 ng(r=0.9998)、4.26~29.82 ng(r=0.9999)、49.26~492.6 ng(r=0.9999)、9.86~98.6 ng(r=1.0000);平均回收率及RSD均符合药典规定。结论所建方法专属性强,重复性好,可用黄连上清片的质量控制。Objective To establish a method to simultaneously determine 12 compounds in Huanglian Shangqing pills by HPLC combined with wavelength switching method. Methods The chromatograhic column was Welch-Ultimate-C_（18）（4.6 mm×250 mm, 5 μm）; the column temperature was maintained at 30 ℃; A linear elution of 0.3% phosphoric acid aqueous solution acetonitrile was adopted at 1 m L·min（-1）. The. UV detection wavelength was switched. Results Phellodendrine, lliquiritin, baicalin, berberine, baicalein, aloeemodin, rhein, imperatorin, emodin, isoimperatorin, chrysophanol, and physcion had good linearity at 248- 1736 ng（r =0.9996）, 82.94- 580.58 ng（r = 1.0000）, 68.54- 685.4 ng（r = 0.9999）, 33.8- 236.6 ng（r = 0.9996）, 149.6- 1047.2 ng（r = 0.9999）, 31.54- 220.78 ng（r = 1.0000）, 27.74- 267.4 ng（r = 0.9998）, 7.68-53.76 ng（r = 0.9999）, 32.84- 229.88 ng（r = 0.9998）, 4.26- 29.82 ng（r = 0.9999）, 49.26- 492.6 ng（r= 0.9999） and 9.86- 98.6 ng（r = 1.0000）, respectively. The average recoveries all meet the requirements of Pharmacopoeia. Conclusion This method is simple accurate and reproduceable, which can be used for the quality control of Huanglian Shangqing pill.

关 键 词：黄连上清丸 高效液相色谱法 黄柏碱 甘草苷 黄芩苷 小檗碱 黄芩素 芦荟大黄素 大黄酸 欧前胡素 大黄素 异欧前胡素 大黄酚 大黄素甲醚 

分 类 号：R917[医药卫生—药物分析学]