注射用醋酸亮丙瑞林微球中的聚乙烯醇(PVA)残留量测定

Determination of Polyvinyl Alcohol Residue in Leuprorelin Acetate Microsphere for Injection

目的建立了高效液相色谱法测定注射用醋酸亮丙瑞林微球中的聚乙烯醇(PVA)残留量。方法采用凝胶色谱柱(Agilent PL aquagel-OH 40,300 mm×7.5 mm,8μm);水作为流动相,流速为1.0 mL·min^(-1);示差折光检测器(RID),检测器温度为25℃;进样量为10μL。结果空白溶剂、微球中的原料及辅料对PVA测定没有干扰;PVA在0.203~1.217 mg·mL^(-1)(20%~150%)的浓度范围内线性良好(相关系数r=0.9999),线性方程y=104661.217x-209.11,y轴截距为100%响应值的0.2%;PVA的定量限为40.6μg·mL^(-1),检测限为10.0μg·mL^(-1);重复测定6次,PVA含量测定结果的平均值为10.56 mg,RSD为0.9%;在80%~120%范围内的回收率均在98%~102%之间,平均回收率为100.6%(n=9)(RSD=1.1%,n=9)。结论该方法专属性高、重复性好、准确度高、可以用于注射用醋酸亮丙瑞林微球中的PVA残留量测定。

OBJECTIVE To establish a method for the determination of polyvinyl alcohol(PVA)residuesin leuprorelin acetate microsphere for injection.METHODS High performance liquid chromatography(HPLC)was adopted.The determination was performed on Agilent PL aquagel-OH 40 column(300 mm×7.5 mm,8μm)using refractive index detector(RID)with temperature of 25℃.The mobile phase was water and the flow rate was 1.0mL·min^(-1).The injection volume was 10μL.RESULTS PVA had good linear relationship between 0.203-1.217 mg·mL^(-1)(20%-150%)with linear equation of y=104661.217x-209.11(r=0.9999).The blank solution,raw materials and accessories did not interfere the determination of PVA.The limits of quantitation and detection were 40.6μg·mL^(-1) and 10.0μg·mL^(-1) respectively.The average content of PVA in repeatability tests(n=6)was 10.56 mg(RSD=4%)and the recovery wasreached 98%to 102%within the range from 80%-120%.The average recovery was 100.6%(RSD=1.1%,n=9).CONCLUSION Themethod has goodspecificity,good repeatability and high accuracy.It can be used to determine PVA residues in leuprorelin acetate microsphere for injection.