论文部分内容阅读
目的:测定尿液中苯乙醛酸和苯乙醇酸含量。方法:采用Kromasil C18柱(250 mm×4.6 mm,5μm);流动相为乙腈-混合酸(冰醋酸0.5 mL+磷酸0.5 mL+水1000 mL)(5∶95),流速为1 mL.min-1,柱温为25℃,检测波长为225 nm。结果:本实验对190个样品进行测定,PGA含量为0~0.384 mg.mL-1,平均含量为0.071 mg.mL-1;MA含量为0.007~0.497 mg.mL-1,平均含量为0.121 mg.mL-1。本方法苯乙醛酸在0.03298~0.4122 mg.mL-1(r=0.9991)范围内峰面积与浓度线性关系良好,定量限为17.2 ng;样品的加标回收率为95.2%~104.3%;批内精密度RSD为4.3%~6.8%,批间精密度RSD为4.5%~8.7%。苯乙醇酸在0.08158~1.0198 mg.mL-1(r=0.9994)范围内峰面积与浓度线性关系良好,定量限为20.4 ng;样品的加标回收率为99.3%~104.2%,批内精密度RSD为3.0%~5.1%,批间精密度RSD为5.7%~9.8%。结论:本方法操作简便,适用于尿中苯乙醛酸和苯乙醇酸的含量测定。
Objective: To determine the content of phenylglyoxylic acid and mandelic acid in urine. Methods: Kromasil C18 column (250 mm × 4.6 mm, 5 μm) was used. The mobile phase was acetonitrile-mixed acid (0.5 mL of glacial acetic acid + 0.5 mL of phosphoric acid + 1000 mL of water) The column temperature was 25 ℃ and the detection wavelength was 225 nm. Results: 190 samples were assayed in this experiment. The average PGA content was 0 ~ 0.384 mg.mL-1, the average content was 0.071 mg.mL-1, the MA content was 0.007 ~ 0.497 mg.mL-1, the average content was 0.121 mg .mL-1. The linear range of the peak area and concentration of phenylglyoxylic acid in the range of 0.03298 ~ 0.4122 mg.mL-1 (r = 0.9991) was good with the limit of quantification of 17.2 ng and the spiked recoveries of 95.2% -104.3% The internal precision RSD was 4.3% ~ 6.8%, and the inter-batch precision RSD was 4.5% ~ 8.7%. The linear range of peak area to concentration of mandelic acid was 0.08158 ~ 1.0198 mg.mL-1 (r = 0.9994). The limit of quantification was 20.4 ng. The spiked recoveries were 99.3% -104.2%. The intra-assay precision RSD was 3.0% ~ 5.1%, inter-batch precision RSD was 5.7% ~ 9.8%. Conclusion: The method is simple and easy to operate and is suitable for the determination of phenylglyoxylic acid and mandelic acid in urine.