HPLC波长切换法测定伸筋丹胶囊中柚皮苷、4-甲氧基水杨醛和山奈素的含量

Determination of Naringin 4-methoxy Salicylaldehyde kaempferide in Shenjin Dan Capsules by HPLC with UV Switch

目的:建立高效液相色谱(HPLC)法同时测定伸筋丹胶囊中柚皮苷、4-甲氧基水杨醛和山奈素3个成分的含量。方法:采用BDS-HYPERSIL C18色谱柱(4.6 mm×250 mm,5μm),以乙腈-1%冰乙酸为流动相,梯度洗脱,流速1 mL·min^(-1),检测波长283 nm(0~10 min,测定柚皮苷)、278 nm(10~16.5 min,测定4-甲氧基水杨醛)、360 nm(16.5~30 min,测定山奈素)。结果:各待测成分分离度良好,柚皮苷、4-甲氧基水杨醛、山奈素的进样量分别在7.93~158.6 ng、6.85~137 ng、3.2~64 ng范围内与峰面积呈良好的线性关系;加样回收率分别为101.2%(RSD=1.0%)、99.3%(RSD=0.8%)、98.1%(RSD=1.5%)。结论:HPLC法简单、快速、灵敏、准确,可用于伸筋丹胶囊中柚皮苷、4-甲氧基水杨醛和山奈素的含量测定。

Objective： To develop an HPLC method for simultaneous determination of naringin 4-methoxy salicylaldehyde kaempferide in Shenjin dan capsules. Methods： The chromatographic separation was carried out on a BDS-HYPERSIL C18 column （4. 6 mm x 250 mm,5 Ixm） with a mobile phase consisting of acetonitrile-l% glacial acetic acid in a gradient mode at a flow rate of 1 mL - min-1. The UV detection wavelength was set at 283 nm for naringin in the first 10 min ,278 nm for 4-methoxy salicylaldehyde during 10 - 16. 5 min, 360 nm for kaempferide during 16. 5 - 30 min. Results： Excellent chromatographic separation was achieved and the ranges for linear cor- relation of naringin 4-methoxy salicylaldehyde kaempferide were 7. 93 - 158. 6 ng（r2 =0. 9987）, 6. 85 - 137 ng（r2 =0. 9999） and 3. 2 - 64 ng（ r2 = 0. 9990 ） , respectively. The average recoveries of the three components were 101.2% （ RSD = 1.0% ） , 99. 3% （ RSD = 0. 8% ） and 98. 1% （RSD = 1.5 % ）. Conclusion： The established method is simple,rapid, sensitive and accurate, which can be applied to determine naringin 4-methoxy salicylaldehyde kaempferide in Shenjin dan capsules.