摘要
目的建立快速、灵敏的液相色谱-串联质谱法测定人血浆中倍他米松(BOH)浓度的方法。方法采用Agilent Zorbax C_(18)(2.1mm×150mm,5μm)色谱柱,柱温25℃,流动相为甲醇-水(85:15,V/V),流速为0.2mL·min^(-1),电喷雾(ESI)离子源,多反应离子监测(MRM)的扫描方式。BOH采用负离子检测,二丙酸倍氯米松(内标,IS)采用正离子检测,BOH和IS的离子通道分别选择为m/z 361.0→m/z307.2和m/z 543.1→m/z 433.2。结果 BOH在0.1～30μg·L^(-1)浓度范围内有良好的线性关系(r^2=0.999 1),定量下限(LOQ)为0.1μg·L^(-1),日内、日间精密度(RSD)均小于15%,提取回收率均在65%左右,相对回收率均在85%～115%范围内。结论该方法简便、准确、灵敏,可用于人血浆中BOH的浓度检测、人体药动学和生物等效性研究。
AIM To establish a sensitive and fast liquid chromatography tandem mass spectrometric method for the determination of betamethasone in human plasma.METHODS Agilent Zorbax C_（18）（2.1 mm×150 mm,5μm）chromatographic column were employed to determine the concentration of betamethasone in human plasma.Column temperature was 25℃.The mobile phase consisted of methanol-water（85：15,V/V） and flow rate was 0.2 mL·min^（-1）.The ions of analyte were detected by multiple ionic reaction monitoring mode （MRM）.A tandem mass spectrometer equipped with electrospray ionization source was used as the detector operating in negative ion mode for betamethasone and positive ion mode for beclomethasone dipropionate （internal standard,IS）,and the mass transition pairs of m/z 361.0→m/z 307.2 and m/z 543.1→m/z 433.2 were used to detect betamethasone and IS respectively.RESULTS The standard curve of betamethasone was linear over the concentration range of 0.1-30μg？L^-1（r^2=0.9991）.The limit of qualification of betamethasone was 0.1μg·L^-1.Within-day RSD and between-day RSD were less than 15%,and the extraction recovery rate was about 65%and the relative recovery were all within 85%-115%.CONCLUSION This method is simple,accurate and sensitive.It can be used for the determination of betamethasone concentration in human plasma,clinical pharmacokinetics and bioequivalence studies.
出处
《中国新药与临床杂志》
CAS
CSCD
北大核心
2011年第3期220-225,共6页
Chinese Journal of New Drugs and Clinical Remedies
关键词
倍他米松
色谱法
高压液相
光谱法
质量
电喷雾电离
betamethasone
chromatography
high pressure liquid
spectrometry
mass
electrospray ionization
