反相高效液相色谱法测定尿液中己内酰胺

Analysis of caprolactam in urine by reversed phase high-performance liquid chromatography

目的建立尿中己内酰胺的反相高效液相色谱测定方法。方法尿液经乙腈沉淀,稀释定容后以5000 r/min高速离心,取上清液过0.45μm微孔滤膜后上机测定,采用Sunfire C18色谱柱分离,以乙腈-水(10:90,V/V)为流动相,在210 nm波长下紫外检测器检测。结果己内酰胺标准浓度为0 mg/L~200 mg/L时,线性关系良好(r=0.9999),方法定量限为0.42 mg/L,加标回收率为95.4%~106.1%,相对标准偏差(RSD)为1.8%~4.6%。在优化色谱条件下,多种酰胺类化合物均不干扰己内酰胺的测定。结论本方法简便、快速,灵敏度、准确度高,适于尿液中己内酰胺的测定。

Objective To establish a method for the determination of caprolactam in urine by reversed phase high-performance liquid chromatography(RP-HPLC).Methods The urine was diluted with acetonitrile and centrifuged at high speed of 5000 r/min.The supernatant was determined after filtration with 0.45μm microporous membrane.It was separated by Sunfire C18 column.Acetonitrile-water(10:90,V/V)was used as mobile phase and detected by UV detector at 210 nm.Results Good linearity was obtained when the concentration of caprolactam was within 0 mg/L-200 mg/L(r=0.9999).The quantification limit was 0.42 mg/L.And the range of recovery rates at three levels was within 95.4%-106.1%,with the relative standard deviations of 1.8%-4.6%.Under the optimized chromatographic conditions,several amide compounds did not interfere with the determination of caprolactam.Conclusion The method shows advantages in efficiency,high sensitivity and accuracy,and it is suitable for analysis of caprolactam in urine.