Department of Chemistry, Faculty of Science, Universiti Putra Malaysia, Serdang, Selangor, Malaysia.
Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, Johor Bahru, Johor, Malaysia.
J Sep Sci. 2017 Nov;40(21):4222-4233. doi: 10.1002/jssc.201700549.
A new facile magnetic micro-solid-phase extraction coupled to gas chromatography and mass spectrometry detection was developed for the extraction and determination of selected antidepressant drugs in biological fluids using magnetite-MCM-41 as adsorbent. The synthesized sorbent was characterized by several spectroscopic techniques. The maximum extraction efficiency for extraction of 500 μg/L antidepressant drugs from aqueous solution was obtained with 15 mg of magnetite-MCM-41 at pH 12. The analyte was desorbed using 100 μL of acetonitrile prior to gas chromatography determination. This method was rapid in which the adsorption procedure was completed in 60 s. Under the optimized conditions using 15 mL of antidepressant drugs sample, the calibration curve showed good linearity in the range of 0.05-500 μg/L (r = 0.996-0.999). Good limits of detection (0.008-0.010 μg/L) were obtained for the analytes with good relative standard deviations of <8.0% (n = 5) for the determination of 0.1, 5.0, and 500.0 μg/L of antidepressant drugs. This method was successfully applied to the determination of amitriptyline and chlorpromazine in plasma and urine samples. The recoveries of spiked plasma and urine samples were in the range of 86.1-115.4%. Results indicate that magnetite micro-solid-phase extraction with gas chromatography and mass spectrometry is a convenient, fast, and economical method for the extraction and determination of amitriptyline and chlorpromazine in biological samples.
采用磁铁矿-介孔硅 MCM-41 为吸附剂，建立了一种新的简便磁微固相萃取方法，结合气相色谱和质谱检测，用于从生物体液中萃取和测定选择的抗抑郁药物。通过多种光谱技术对合成的吸附剂进行了表征。在 pH 12 时，从水溶液中萃取 500μg/L 的抗抑郁药物，最大萃取效率为 15mg 磁铁矿-MCM-41。在气相色谱测定前，用 100μL 乙腈解吸分析物。该方法快速，吸附过程在 60s 内完成。在优化条件下，使用 15mL 抗抑郁药物样品，校准曲线在 0.05-500μg/L 范围内具有良好的线性（r=0.996-0.999）。对于分析物，检测限良好（0.008-0.010μg/L），相对标准偏差<8.0%（n=5），用于测定 0.1、5.0 和 500.0μg/L 的抗抑郁药物。该方法成功应用于测定血浆和尿液中的阿米替林和氯丙嗪。加标血浆和尿液样品的回收率在 86.1-115.4%范围内。结果表明，采用气相色谱和质谱法的磁铁矿微固相萃取是一种方便、快速、经济的方法，用于从生物样品中萃取和测定阿米替林和氯丙嗪。
