摘要
目的:建立LC-ESI-MS法测定大鼠体内的同型半胱氨酸(HCY)。方法:色谱柱为Zorbax SB-C18(2.1mm×100mm,3.5μm),乙腈-水(40∶60)为流动相,流速为0.3mL·min-1,柱温为30℃。ESI(电喷雾离子源),正离子检测,雾化气压力设为172.375kPa;干燥气(N2)流速设为7L·min-1,干燥气温度设为350℃,[M+H]+,m/z136。结果:HCY在2.5~100μmol.L-1范围内线性关系良好,线性方程C=0.0079X-8.1011,r=0.9981,最低检测限为1μmol.L-1。HCY日内及日间精密度RSD均低于6%。12周龄的Wistar-Kyoto大鼠,自发性高血压大鼠体内HCY的浓度分别为(9.57±3.49)μmol.L-1和(11.59±3.13)μmol.L-1。结论:该法操作简便、快速,灵敏度高,可用于大鼠体内HCY的检测。
Objective:To establish an LC-ESI-MS method for determination of homocysteine in rat plasma.Methods:A Zorbax SB-C18(2.1 mm×100 mm,3.5 μm)column was used,with mobile phase of methanol-water(40∶60),flow rate 0.3 mL·min-1,column temperature 30 ℃.Electrospray ionization(ESI)source was applied and operated in positive ion mode.The pressure of atomizing gas set up 172.375 kPa;the flow rate of drying gas(N2)was 7 L·min-1 and the temperature was 350 ℃,[M+H]+,m/z 136.Results:The calibration curve of homocysteine in plasma was linear in the concentration range of 2.5-100 μmol·L-1.C= 0.0079X-8.1011,r=0.9981.The LLOQ was 1 μmol·L-1.The precision of intra-day and inter-day was both below 6%.The concentration of HCY in 12 weeks Wistar-Kyoto and SHR(Spontaneously hypertensive rats)were(9.57±3.49)μmol·L-1 and(11.59±3.13)μmol·L-1,respectively.Conclusion:The analytical method for homocysteine is accurate,sensitive and suitable for analysis of rat plasma concentration.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2010年第12期2267-2269,共3页
Chinese Journal of Pharmaceutical Analysis