摘要
建立了利用高效液相色谱仪快速测定脑蛋白水解物注射液中氨基酸含量的方法。样品处理采用先提取后水解转化的方法,色谱分离使用反相C18分析柱二元高压梯度洗脱;使用二极管阵列检测器检测,波长为260 nm;分析时间为14 min。各氨基酸在4.5~900μmol/L范围内线性关系良好,相关系数为0.9987~0.9999;检出限为0.032~0.578 mg/L,定量限为0.105~1.929 mg/L;16种氨基酸回收率为95.39%~105.33%,日内和日间分析的相对标准偏差(n=7)分别为1.95%~4.81%和3.14%~6.70%。
A HPLC for rapid determination of amino acids in cerebroprotein hydrolysate injection was developed. Norvaline was added to samples before preparation as internal standard. Then online derivatization with o-phthaldialdehyde(OPA) and 9-fluore- nylmethyl ehloroformate( FMOC - C1) was performed automatically by the autosampl.er, and analyzed on a Cas short column using gradi- ent elution with diode array detector( for lysine) and fluorescence detector( for other amino acids except lysine) combined detection. The analytical time was 14 min. The peak area of amino acids versus their concentration had a good linearity ( correlation coefficients were 0.998 7 - 0. 999 9 ) in the range of 4.5 - 900 μmol/L. limits of detection(LOD) were in the range of 0.032 - 0.578 mg/L, lim- its of quantification(LOQ) were in the range of 0. 105 - 1. 929 mg/L. The recoveries of standard spiking old6 amino acids were in the range of 95.39% -105.33%. The relative standard deviations( n = 7) of intraday and interday were in the range of 1.95% -4.81% and 3.14% - 6.70%, respectively.
出处
《化学分析计量》
CAS
2011年第5期29-33,共5页
Chemical Analysis And Meterage