高效液相色谱法测定聚乙烯吡咯烷酮

Determination of Polyvinylpyrrolidone by High Performance Liquid Chromatography

聚乙烯吡咯烷酮(PVP)是一种具有天然表面活性的多功能聚合物,由于其分子量分布范围广,两亲性强,很难准确定量测定。本研究建立了高效液相色谱(HPLC)检测K85-聚乙烯吡咯烷酮的定量分析方法,并对色谱检测条件进行了优化。该分析方法使用Inertsil ODS-SP C_(18)柱(250 mm×4.6 mm,5 μm),流动相为乙腈与水的混合液(10∶90,v∶v),流速为1.0 mL/min,检测波长为205 nm。运用所建立的方法进行测定时,将聚合物解析为单峰,出峰时间t_R=(5.705±0.005)min。检测过程中,色谱柱性能保持不变,峰形保持良好。在5~100 μg/mL呈现良好的线性关系(R^(2)=0.998 8,n=5),检测限为18.9 ng/mL,定量限为57 ng/mL。3次平行添加实验显示,平均回收率分别为99.50%、99.99%、100.64%,RSD值分别为0.996%、0.857%、0.674%。该方法适用于PVP从聚砜类透析膜上洗脱量的相关测定。

Polyvinylpyrrolidone(PVP)is a versatile polymer with innate surface activity.It is very difficult to accurately determine the quantity of PVP due to its wide molecular weight range and amphiphilic nature.In this study,an analytical method for the quantitative detection of K85-PVP by high performance liquid chromatography(HPLC)is established,and the chromatographic conditions are optimized.The described analytical method uses an Inertsil ODSSP C18 column(250 mm×4.6 mm,5μm),a mixture of acetonitrile and water as the mobile phase(10∶90,v∶v),with a flow rate of 1.0 mL/min and a detection wavelength of 205 nm.During the determination,the polymeris resolved into a single peak,establishing the peak time tR=(5.705±0.005)min.Throughout the detection and research process,the performance of the chromatographic column remained unchanged and the peak shape remained good.A good linear relationship exists in the concentration range of 5~100μg/mL(R^(2)=0.9988,n=5),with the detection limit 18.9 ng/mL and the quantification limit 57 ng/mL.Three parallel additional experiments show that the average recoveries are 99.50%,99.99%,100.64%,and the RSD values are 0.996%,0.857%,0.674%,respectively.The method herein described is suitable for the quantitative determination of the elution volume of PVP from polysulfone type dialysis membranes.