Ma Wei, Ma Qiang, Fu Li, Ma Liqing, Wang Haibo, Liu Caiyun, Tang Yingzhang
Dongning Entry-Exist Inspection and Quarantine Bureau, Dongning 157200, China.
Se Pu. 2010 Jan;28(1):43-8. doi: 10.3724/sp.j.1123.2010.00043.
A sensitive and selective analytical method based on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has been developed for the simultaneous determination of rimonabant and orlistat in weight-loss functional foods. After the foods were extracted under accelerated solvent extraction, the HPLC separation was performed on a Waters Atlantis T3 column (150 mm x 2.1 mm, 3 microm) with a linear gradient elution program of methanol and 10 mmol/L ammonium acetate as the mobile phase. Electrospray ionization was applied and operated in the positive ion mode. The results showed that the limits of detection for the rimonabant and orlistat were 0.5 mg/kg. The calibration curves showed good linearities for rimonabant and orlistat in the range of 0.5 - 100 microg/L, and the correlative coefficients were 0.998 9 and 0.999 4, respectively. The mean recoveries at the 3 spiked levels (2, 5, 10 mg/kg) were 80.5% - 102.1% with the intra-day precision less than 6% and the inter-day precision less than 8%. The work studied the mass spectrum characterization of the 2 drugs and speculated on the fragmentation pathways. The method is sensitive, reproducible and adapts to the determination of rimonabant and orlistat in different weight-loss functional foods.
已开发出一种基于高效液相色谱-串联质谱法(HPLC-MS/MS)的灵敏且选择性高的分析方法,用于同时测定减肥功能食品中的利莫那班和奥利司他。食品经加速溶剂萃取后,采用沃特世Atlantis T3色谱柱(150 mm×2.1 mm,3μm)进行HPLC分离,以甲醇和10 mmol/L醋酸铵为流动相进行线性梯度洗脱程序。采用电喷雾电离并在正离子模式下运行。结果表明,利莫那班和奥利司他的检测限均为0.5 mg/kg。校准曲线表明,利莫那班和奥利司他在0.5 - 100μg/L范围内具有良好的线性关系,相关系数分别为0.998 9和0.999 4。在3个加标水平(2、5、10 mg/kg)下的平均回收率为80.5% - 102.1%,日内精密度小于6%,日间精密度小于8%。该研究工作对这2种药物的质谱特征进行了研究,并推测了裂解途径。该方法灵敏、可重现,适用于不同减肥功能食品中利莫那班和奥利司他的测定。