LC-MS法测定人血浆中尼美舒利的浓度

目的:建立以液-质联用法测定人血浆中尼美舒利浓度的方法。方法:色谱柱为Agilent Zorbox SB-Cl8,流动相为乙腈-0.1%甲酸(65∶35),流速为1.0mL·min-1,柱温为35℃,内标为缬沙坦;正离子检测模式,选择m/z309(尼美舒利,M+H]+)和m/z436(缬沙坦,M+H]+)进行监测。结果:尼美舒利血药浓度在5～50ng·mL-1范围内线性关系良好(r=0.9989);方法回收率为87.1%～92.9%;日内、日间RSD分别为3.1%～5.8%、6.4%～9.2%。结论:本方法灵敏、简便,结果准确可靠,重复性好,可用于尼美舒利的临床血药浓度监测和药动学研究。

Determination of Nimesulide in Human Plasma by LC-MS

OBJECTIVE： To establish an LC-MS method for the determination of nimesulide in human plasma. METHODS： The separation was performed on Agilent Zorbox SB-C18 column, using acetonitrile -0.1% formic acid （65：35） as the mobile phase at a flow rate of 1.0 mL-min^-1. The column temperature was set at 35 ℃ and valsartan was served as internal standard. Positive electrospray ionization detection was applied to monitor m/z 309 （nimesulide, M＋H]＋） and m/z 436 （valsartan, M＋H]~）. RE- SULTS： The linear range of nimesulide was 5-50 ng-mL^-1（r= 0.998 9）. The method recovery of nimesulide ranged from 87.1% to 92.9%. The intra-day and inter-day RSD were 3.1%-5.8%, 6.4%-9.2%, respectively.CONCLUSION： The method is sensitive, simple, convenient, accurate and reproducible, and it is suitable for clinical plasma concentration monitoring and pharmacokinetics research of nimesulide.