White Lyndsey, Ma Jing, Liang Su, Sanchez-Espiridion Beatriz, Liang Dong
Department of Pharmaceutical and Environmental Health Sciences, Texas Southern University, Houston, TX 77004, United States.
Department of Epidemiology, The University of Texas MD Anderson Cancer Center, Houston, TX 77030, United States.
J Pharm Biomed Anal. 2017 Apr 15;137:54-59. doi: 10.1016/j.jpba.2016.12.017. Epub 2016 Dec 28.
Several metabolites in human serum have been identified as potential cancer biomarkers for early detection. This study focuses on the LC-MS/MS method development and validation of d-mannose in human serum. Surrogate blank serum, coupled with stable isotope d-mannose-C, as internal standard, was used for generating standard curves ranging from 1 to 50μg/mL. Separation was achieved by an Agilent 1200 series HPLC equipped with a SUPELCOGELTM Pb, 6% Crosslinked column with HPLC water as a mobile phase at flow rate of 0.5mL/min at 80°C. Mass detection was performed under negative ionization electrospray. Inter- and intra-day accuracy and precision were <2%. The extraction recovery and matrix effect were 104.1%-105.5% and 97.0%-100.0%, respectively. This method was successfully applied for the quantification of d-mannose in the serum samples of 320 esophageal cancer patients and 323 healthy volunteers. We report a simple, specific and reproducible LC-MS/MS method for the quantification of d-mannose in human serum as a potential cancer biomarker.
人血清中的几种代谢物已被确定为早期检测潜在的癌症生物标志物。本研究聚焦于液相色谱-串联质谱法（LC-MS/MS）检测人血清中D-甘露糖的方法开发与验证。以替代空白血清并结合稳定同位素D-甘露糖-C作为内标，用于生成浓度范围为1至50μg/mL的标准曲线。采用配备SUPELCOGELTM Pb、6%交联柱的安捷伦1200系列高效液相色谱仪进行分离，以高效液相色谱水为流动相，在80°C下以0.5mL/min的流速进行。在负离子电喷雾模式下进行质谱检测。日间和日内准确度及精密度均<2%。提取回收率和基质效应分别为104.1%-105.5%和97.0%-100.0%。该方法成功应用于320例食管癌患者和323例健康志愿者血清样本中D-甘露糖的定量分析。我们报道了一种简单、特异且可重复的LC-MS/MS方法，用于定量分析人血清中的D-甘露糖作为潜在的癌症生物标志物。
