反相离子对HPLC同时测定制马钱子中4种生物碱的含量  

Simultaneous Determination of Four Alkaloids in Processed Semen Strychni by Ion Pair RP-HPLC

作　　者：刘学湘[1] 潘扬[1] 王丽[1] 刘亮镜[1] 

机构地区：[1]南京中医药大学药用菌与中药生物技术研究所,南京210029

出　　处：《中国药学杂志》2010年第9期698-702,共5页Chinese Pharmaceutical Journal

基　　金：2010版国家药典项目(YD-085);青蓝工程(2008年)项目

摘　　要：目的建立同时测定制马钱子中4种生物碱士的宁、马钱子碱、士的宁氮氧化物、马钱子碱氮氧化物含量的反相离子对HPLC法。方法应用Lichrospher S C18色谱柱(4.6mm×300mm,5μm),以乙腈-水(38:62,每1000mL加入磷酸二氢钾3.4g和十二烷基硫酸钠1.7g)为流动相,流速:1.0mL.min-1,柱温:30℃,检测波长:260nm。结果4种生物碱士的宁、马钱子碱、士的宁氮氧化物和马钱子碱氮氧化物的线性范围分别为13.7～219.1,12.55～200.8,0.3743～5.988和0.6225～9.96mg.L-1(r>0.9999),平均回收率分别为98.0%,102.2%,103.3%和99.9%(RSD均小于2.5%)。结论该方法简便、准确,重复性好,适用于制马钱子中士的宁、马钱子碱、士的宁氮氧化物、马钱子碱氮氧化物的含量测定。OBJECTIVE To develop an ion pair RP-HPLC method for determining the contents of four alkaloids,including strychnine,brucine,strychnine N-oxide and brucine N-oxide in processed Semen Strychni.METHODS The analysis was performed on a Lichrospher S C18 column （4.6 mm×300 mm,5 μm）.The mobile phase was a mixture of acetonitrile and water （38：62）,with the addition of 3.4 g monopotassium phosphate （KH2PO4） and 1.7 g sodium dodecyl sulfate （SDS） as an ion pair per 1 000 mL.The flow rate was 1.0 mL·min-1,the column temperature was at 30 ℃ and the detection wavelength was at 260 nm.RESULTS The linear ranges of strychnine,brucine,strychnine N-oxide and brucine N-oxide were 13.7-219.1,12.55-200.8,0.3743-5.988 and 0.622 5-9.96 mg·L^-1,respectively （r〉0.999 9）.Their average recoveries were 98.0%,102.2%,103.3% and 99.9% （RSD all less than 2.5%）,respectively.CONCLUSION The method is simple,accurate and reproducible,and can be used for simultaneous determination of strychnine,brucine,strychnine N-oxide and brucine N-oxide in processed Semen Strychni.

关 键 词：反相离子对高效液相色谱法 制马钱子 士的宁 马钱子碱 士的宁氮氧化物 马钱子碱氮氧化物 

分 类 号：R284[医药卫生—中药学]