RP-HPLC法测定枳壳中5个脂溶性成分的含量

RP-HPLC determination of five lipophilic components in Fructus Aurantii

目的:建立RP-HPLC测定枳壳中水合橙皮内酯、马尔敏、川陈皮素、桔皮素和橙皮油素的含量。方法:采用DiamonsilC18(150mm×4.6mm,5μm)色谱柱,流动相为甲醇(A)-水(B),梯度洗脱(0～7min,51%A;7～9min,51%A→59%A;9～14min,59%A→60%A;14～15min,60%A→64%A;15～25min,64%A;25～29min,64%A→95%A;29～30min,95%A→100%A;30～36min,100%A),流速1.0mL.min-1,检测波长324nm,柱温30℃。结果:5个成分均能获得基线分离,水合橙皮内酯、马尔敏、川陈皮素、桔皮素和橙皮油素进样量分别在0.0855～2.052,0.0341～0.819,0.0414～0.993,0.0416～0.998,0.0408～0.978μg范围内呈良好的线性关系;平均回收率(n=6)分别为99.11%(RSD=0.59%),101.1%(RSD=2.6%),99.52%(RSD=0.85%),99.59%(RSD=0.95%),97.44%(RSD=1.6%)。结论:该法简便快速,重现性好,准确可靠,可作为枳壳药材及饮片中水合橙皮内酯、马尔敏、川陈皮素、桔皮素和橙皮油素5个脂溶性成分测定的有效方法。

Objective：To establish an RP-HPLC method for simultaneous determination of meranzin hydrate,marmin,nobiletin,tangeretin and auraptene in Fructus Aurantii.Methods：Five lipophilic constituents were separated with Diamonsil C18 （150 mm×4.6 mm,5 μm） column with a flow rate of 1.0 mL·min-1 at 30 ℃ and detected at 324 nm. Mobile phase consisted of methanol（A） and water（B） with gradient elution（0-7 min,51%A;7-9 min,51%A→59%A;9-14 min,59%A→60%A;14-15 min,60%A→64%A;15-25 min,64%A;25-29 min,64%A→95%A;29-30 min,95%A→100%A;30-36 min,100%A）.Results：Five liposoluble constituents were well separated.The linear ranges for meranzin hydrate,marmin,nobiletin,tangeretin and auraptene were 0.0855-2.052,0.0341-0.819,0.0414-0.993,0.0416-0.998,0.0408-0.978 μg,respectively;The mean recoveries（n=6） were 99.11%（RSD=0.59%）,101.1%（RSD=2.6%）,99.52%（RSD=0.85%）,99.59%（RSD=0.95%）,97.44%（RSD=1.6%）,respectively.Conclusion：This method is simple,reproducible,accurate,reliable for determination of meranzin hydrate,marmin,nobiletin,tangeretin and auraptene in Fructus Aurantii.