RP-HPLC法测定枳壳中5个脂溶性成分的含量

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Diamonsil C₁₈(150 mm×4.6 mm,5 μm)色谱柱,流动相为甲醇(A)-水(B),梯度洗脱(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),流速1.0 mL·min^-1,检测波长324 nm,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0.0855~2.052,0.0341~0.819,0.0414~0.993,0.0416~0.998,0.0408~0.978 μg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.