Quantification of 8-iso-prostaglandin-F2α and 2,3-dinor-8-isoprostaglandin-F2α in human urine using liquid chromatography-tandem mass spectrometry
Quantification of 8-iso-prostaglandin-F2α and 2,3-dinor-8-isoprostaglandin-F2α in human urine using liquid chromatography-tandem mass spectrometry
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DOI：
10.1016/s0891-5849(02)01018-3
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发表时间：
2003-02-15
影响因子：
7.4
通讯作者：
Heward, CB
中科院分区：
文献类型：
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作者：
Liang, YL;Wei, P;Heward, CB
8-异前列腺素F-2α(8-iso-PGF(2α))的定量被认为是脂质过氧化的可靠指标，可能与体内自由基的产生、氧化损伤和抗氧化剂缺乏有关。建立了人尿样中8-异-前列腺素F-2α(2-iso-PGF，2α)及其代谢物2，3-dior-8-iso-prostaglandin F-2α(2，3-dior-8-iso-PGF(2α))的LC-MS/MS定量方法。在使用自动C18固相萃取程序进行初步纯化步骤后，尿样被直接注入液相色谱(LC)系统并用串联质谱仪进行检测。方法的检出限分别为9 pg、8-iso-PGF(2α)和3 pg(2α)，日内和日间变异均小于12%。在三个不同水平上，两种分析物的不准确度均小于3%。2，3-dior-8-iso-PGF(2α)的尿排泄率高于8-iso-PGF(2α)，且与母体化合物成比例变化(R=0.70，n=60)。该方法与GCMS重复测定8-iso-PGF(2α)具有良好的线性关系(R=0.97，n=15)。吸烟者8-iso-PGF(2α)和2，3-dior-8-iso-PGF(2α)的平均排泄率显著高于非吸烟者(分别为0.53±-0.37vs.0.25+/-0.15mug/g肌酐，p=0.002和8.90+/-3.8vs.4.6+/-2.6mug/g肌酐，p=0.003)。该方法具有良好的准确性、重复性和高通量，可用于大型临床研究和标准临床实验室。(C)2003年爱思唯尔科学公司。
Quantification of 8-iso-prostaglandin F-2alpha (8-iso-PGF(2alpha)) has been suggested to be a reliable indicator of lipid peroxidation that may be related to in vivo free radical generation, oxidative damage, and antioxidant deficiency. We have developed a LC-MS/MS method to quantify 8-iso- PGF(2alpha) and its dinor metabolite, 2,3-dinor- 8-iso-prostaglandin F-2alpha (2,3-dinor-8-iso-PGF(2alpha)), in human urine samples. After an initial purification step using an automated C18 solid phase extraction procedure, the urine sample was injected directly into a liquid chromatography (LC) system and detected with tandem mass spectrometry. The detection limit of the assay was 9 pg for, 8-iso-PGF(2alpha) and 3 pg for 2,3-dinor-8-iso-PGF(2alpha) with both inter- and intraday variations of less than 12%. The inaccuracies were less than 3% for both analytes at three different levels. The urinary excretion rate of 2,3-dinor-8-iso-PGF(2alpha) was higher than that of 8-iso-PGF(2alpha), and changed in proportion to the parent compound (R = 0.70, n = 60). Values obtained with this method showed good linear correlation to duplicate 8-iso-PGF(2alpha) measurements performed with GCMS (R = 0.97, n = 15). The mean excretion rates of 8-iso-PGF(2alpha) and 2,3-dinor-8-iso-PGF(2alpha) were significantly higher in smokers than in nonsmokers (0.53 +/- 0.37 vs. 0.25 +/- 0.15 mug/g creatinine, p = 0.002 for 8-iso-PGF(2alpha) and 8.9 +/- 3.8 vs. 4.6 +/- 2.6 mug/g creatinine, p = 0.003 for 2,3-dinor-8-iso-PGF(2alpha), respectively). The excellent accuracy, reproducibility, and high throughput of this method should permit it to be used in large clinical studies and standard clinical laboratories. (C) 2003 Elsevier Science Inc.