食品中减肥药氯卡色林的测定方法研究
Research of the Method for the Determination of Lorcaserin in Food
摘要:
建立了一种液质联用测定食品中减肥药氯卡色林的方法。实验优化了液相色谱条件及质谱参数。样品经甲醇提取后,采用Thermo C18 (2.1 mm × 150 mm, 2 μm)色谱柱分离,流动相为乙腈-水(含有10 mmol/L乙酸铵)梯度洗脱,流速0.25 mL/min。柱温为30℃,采用正离子模式的电喷雾质谱检测,多反应选择离子检测(MRM)。氯卡色林在0.001~1 mg/L范围内线性良好,相关系数为0.9994。低、中、高3个添加水平的回收率在81.8%~93.3%之间,RSD小于7%,方法的检出限达到1.0 μg/L。另外采用高效液相色谱法考察了氯卡色林原料中的相关物质,发现不同样品相关物质差别较大。本方法简单、高效、准确,可用于食品及中成药中氯卡色林的测定。
Abstract:
A method for the determination of Lorcaserin, a new weight-loss drug in food, using LC-MS was established in this paper. The conditions of HPLC and mass parameters were optimized. Lorcase-rin was extracted with methanol, and then separated on a Thermo C18 (2.1 mm × 150 mm, 2 μm) column. Mixture of acetonitrile and water (containing 10 mmol/L ammonium acetate) was se-lected as mobile phase, and detected with positive-ion electrospray ionization mass spectrometry (ESI MS) under multiple reaction monitoring (MRM) mode. The flow rate of 0.25 mL/min with the column temperature was 30˚C. Good linear calibration was obtained for 0.001 - 1 mg/L with correlation coefficient as 0.9994. The spiked recoveries were in the range of 81.8% to 93.3% (n = 6). While the relative standard deviations (RSDs) were less than 7%, the detection limit of Lorcaserin was 1.0 μg/L. The method was proved to be simple, efficient and accurate, and it could be applied to the detection of Lorcaserin in foods and Chinese patent medicine.
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