反相离子对HPLC同时测定制马钱子中4种生物碱的含量

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。

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

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.