HPLC测定多柔比星壳寡糖硬脂酸胶团中药物的含量

HPLC Determination of Doxorubicin Concentration in Chitosan Oligosaccharide-stearic Acid Micelles

目的采用高效液相色谱法测定壳寡糖硬脂酸嫁接物胶团(CSO-SA)中的多柔比星(DOX)的含量。方法采用Shim-pack VP-ODS色谱柱(150mm×4.6mm,5μm),以0.01mol·L-1的十二烷基硫酸钠溶液-乙腈-甲醇(50∶50∶6)为流动相,内含0.6‰(v/v)的磷酸,流速1.0mL·min-1,检测波长254nm,柱温25℃。结果多柔比星在0.4～8μg·mL-1时,浓度与峰面积呈良好的线性关系,Y=52.926X-3.761(r=0.9999,n=3),定量限为(0.05±0.014)μg·mL-1(S/N>10,n=3)。高、中、低三个浓度的日内RSD为1.82%、0.86%、0.65%,日间RSD为1.73%、0.88%、0.75%,平均加样回收率为(99.38±1.22)%。结论本测定方法操作简便,结果准确。

OBJECTIVE An HPLC analysis method was established for the determination of doxorubicin （DOX） concentration in chitosan oligosaccharide-stearic acid （CSO-SA） micelles. METHODS The segregation and determination of samples were performed on a Shim pack VP-ODS （150 mm ×4.6 mm, 5 μm） column with a mobile phase consisting of 0.01 mol·L^-1 sodium dodecyl sulfate-methanol-acetonitrile （50 ： 50 ： 6） containing 0.6‰ phosphoric acid at a flow-rate of 1.0 mL-min^-1, UV detector was set at 254 nm and column temperature was 25 ℃.RESULTS There was good linear relationship within the range of 0.4-8 μg·mL^-1 of DOX, Y=52.926X-3.761 （r=0.999 9, n=3） . The quantification limit was （0.05±0.014） μg.mL^-1（S/N〉10, n=3）. The RSDs of within-day were 1.82, 0.86, 0.65% ,and the RSDs of between-day were 1.73%, 0.88%, 0.75%, respectively.The average recovery was（99.38 ±.22）%.CONCLUSION The HPLC methods are simple and accurate for the doxorubicin concentration in micellar delivery system.