RP-HPLC法测定壳聚糖微球中5-氟尿嘧啶的包封率

目的建立壳聚糖微球中5氟尿嘧啶包封率的测定方法。方法采用C18色谱柱,甲醇水(体积比为10∶90)为流动相,检测波长266 nm。用超声浸泡研磨法测定了药物的包封率,并与国内外常用的2种测定方法进行对比。结果平均回收率为103.64%,RSD为1.60%(n=5),质量浓度在2.0~20.0 mg.L-1内线性关系良好。测得壳聚糖微球的包封率为42.21%。而其他2种方法测定同一批微球的包封率值比实际偏高或偏低,即测定方法存在问题。结论该法简便灵敏,测得值真实、可靠,适用于交联法制备的壳聚糖微球中药物包封率的测定。

Establishment of drug content determination method in chitosan microspheres

Objective To establish determination method of 5-Fu encapsulation efficiency(EE) in chitosan microspheres(MS) by HPLC.Methods The C_(18) column(15 cm×4.6 mm,5 μm) was used.The mobile phase consisted of methanol-water(V∶V=10∶90) mixture,the detection was set at 266 nm.The ultrasonic-immersing-grinding method was adopted to determine the drug EE.The EE of the same batch MS also ectected with other two methods;methanol-immersing and nitric acid-clearing up respectively.Results The mean recovery was 103.64%,RSD was 1.60%(n=5).The linear range was good in 2.0-20.0 mg·L~(-1).The mean encapsulation efficiency was 42.21%.But the EE detected by methanol-immersing was lower than the true value,the reason was that only the drug on the surface of MS could dissolved.The EE determined by nitric acid-clearing up was higher than the true value,the reason was that some adjuvant had absorption at 266 nm.Conclusions The newly established method is suitable and accurate,which could be developed as the determination method for the drug EE of the chitosan microspheres.