【摘要】 建立了一种专属、灵敏的同时测定血液中咖啡因、盐酸西布曲明等15种减肥药的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。样品经乙腈沉淀后,进入HPLC-MS/MS中分析检测。以甲醇和含0.1%(v/v)冰醋酸的20mmol/L醋酸铵溶液作为流动相,采用梯度洗脱方式,以UltimateXB-C18为色谱柱进行HPLC分析;质谱分析采用电喷雾离子源,正负离子快速切换扫描,选择反应监测模式检测。15种减肥药的定量限在0.001～0.05mg/L内,各种药物的灵敏度较高,各成分的线性相关系数均大于0.99,精密度均小于12.3%,回收率范围为77.3%～110.8%。研究了这15种药物的质谱特征。该方法灵敏、简便、快捷、专属性强,可用于动物实验样品中减肥药物的含量测定,并且对其他药品、食品中目标减肥药物的测定具有借鉴意义。更多还原

【Abstract】 An analytical method for the simultaneous determination of 15 anti-obesity drugs(caffeine,sibutramine,phenformin,etc.) in blood sample was developed using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).After a simple protein precipitation step,the HPLC separation was performed on an UltimateXB-C18 column with methanol and 20 mmol/L ammonium acetate(containing 0.1%(v/v) of glacial acetic acid) as the mobile phases in a gradient elution mode.The MS/MS detection was achieved by electrospray ionization in both positive and negative modes by rapid switching with selective reaction monitoring(SRM).The results showed that the limits of quantification of all anti-obesity drugs were in the range of 0.001-0.05 mg/L.The calibration curves of all anti-obesity drugs showed good linearity and the correlation coefficients were more than 0.99.The recoveries of all anti-obesity drugs at 3 spiked levels were in the range of 77.3%-110.8% with the intra-day and inter-day precisions less than 12.3%.The mass spectrum characterizations of 15 anti-obesity drugs were studied.The method is sensitive and reproducible for the detection of the 15 anti-obesity drugs in blood,and can also be applied to the determination of the anti-obesity drugs in pharmaceuticals or foods.更多还原