高效液相色谱-电喷雾离子阱质谱联用测定尿中的8-羟基脱氧鸟嘌呤

建立了尿样中8-羟基脱氧鸟嘌呤的HPLC-MS测定方法.尿样中的8-羟基脱氧鸟嘌呤采用WCX固相萃取小柱预富集后,以0.5%甲酸-甲醇洗脱,吹干后用0.5 mL流动相溶解剩余物上机测定.采用分子的二级碎片,方法在5.0～500.0 μg/L范围内呈良好线性关系,相关系数r=0.999 4,检出限(S/N=3)为0.50...

Determination of 8-Hydroxy-2'-deoxyguanosine in Urine by High Performance Liquid Chromatography-Electrospray Ionization Trap Mass Spectrometry

A high-performance liquid chromatography-electrospray ionization trap mass spectrometric method was established for the determination of 8-hydroxy-2′-deoxyguanosine(8-OHdG) in urine.The sample was concentrated with WCX cartridge column and eluted out with 0.5%firmic acid-methanol.The elute solution was evaporated to dryness in N2 flow and redissolved with 0.5 mL mobile phase.The analysis of 8-OHdG was carried out using fragment ion of m/z 116 and 167.4 as qualitative ions,and m/z 167.4 as quantitative ion.The method showed good linearity over the range of 5.0-500.0 μg/L for 8-OHdG with a correlation coefficient of 0.999 4.The detection limit(S/N=3) was 0.50 μg/L.The spiked recoveries of 8-OHdG at two concentration levels of 40.0 μg/L and 100.0 μg/L were 82% and 76%,respectively.The proposed method was suitable for the determination of 8-OHdG in urine sample with high selectivity and sensitivity.