摘要
提出了应用气相色谱-质谱法测定血浆中双氯芬酸钠含量。血浆样品中双氯芬酸钠经盐酸提取,并加入三甲基硅烷衍生化试剂进行衍生化,所得衍生化产物经萃取、净化后供气相色谱分离及质谱测定。采用选择离子质谱扫描方式,供试品双氯芬酸钠-三甲基硅烷衍生物定量选择离子检测质荷比为m/z367,内标物布洛芬-三甲基硅烷衍生物定量选择离子检测质荷比为m/z263。双氯芬酸钠的线性范围为0.005～5.0mg·mL-1,检出限(3S/N)为0.5μg.L-1。方法回收率在94.6%～97.4%之间,日内、日间相对标准偏差(n=6)均小于5%。
The method of C-C-MS was applied to the determination of sodium diclofenac in human plasma. The sample containing sodium diclofenac was acidified with HCl and derivatized with trimethylsilane. The derivatized product was extracted and purified, which was then used for GC-MS determination. The selected ion monitoring mode and values of m/z of 367 for diclofenac derivative and m/z of 263 for ibuprofen derivative （internal standrad） were adopted in the MS determination. Linearity range of sodium diclofenac was found between 0. 005- 5.0 mg · L^-1 , with detection limit （3S/N） of 0. 5 μg · L^-1. The values of recovery were found in the range of 94. 6%-97. 4%, with values of intraday and interday RSD＇s less than 5%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2010年第2期153-155,共3页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
