Samanidou Victoria F, Evaggelopoulou Evaggelia N, Papadoyannis Ioannis N
Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, GR-54 124 Thessaloniki, Greece.
J Pharm Biomed Anal. 2005 Jun 1;38(1):21-8. doi: 10.1016/j.jpba.2004.12.005. Epub 2005 Jan 19.
Even nowadays millions of people suffer and even die each year from malaria and hundreds of millions of people especially in tropical countries. Quinine (Q) a natural occurring alkaloid and chloroquine (CQ) a synthetic drug are widely used as anti-malarial agents. Herein an isocratic reversed-phase high performance liquid chromatographic (RP-HPLC) method is described for the simultaneous determination of quinine and chloroquine, at low concentrations, in pharmaceuticals and biological fluids. The present method is characterized by higher sensitivity and analytes are separated in less time than the already published methods. The analytical column, an MZ Kromasil, C18, 5 microm, 250 x 4mm, was operated at ambient temperature with backpressure values of 230 kg/cm(2). Mobile phase consisted of methanol-acetonitrile-0.1 mol/L ammonium acetate, (45:15:40 v/v) at a flow rate of 1.0 mL/min. Fluorescence detection was performed at excitation 325 nm and emission 375 nm, respectively. Salicylic acid was used as internal standard at a concentration of 0.5 ng/microL, resulting in a detection limit of 0.3 ng, while upper limit of linear range was 0.7 ng/microL for quinine and 0.5 ng/microL for chloroquine. Separation was completed within 5 min. The statistical evaluation of the method was examined performing intra-day (n=8) and inter-day calibration (n=8) and was found to be satisfactory, with high accuracy and precision results. Solid phase extraction provided high relative extraction recoveries from biological matrices: 92.1% for quinine and 105.4% for chloroquine from blood serum and 101.8% for quinine and 90.7% for chloroquine from urine.
即使在当今，每年仍有数百万人遭受疟疾折磨甚至死亡，尤其在热带国家，受影响人数达数亿。奎宁（Q）是一种天然生物碱，氯喹（CQ）是一种合成药物，它们被广泛用作抗疟剂。本文描述了一种等度反相高效液相色谱（RP-HPLC）方法，用于同时测定药物和生物流体中低浓度的奎宁和氯喹。本方法具有更高的灵敏度，与已发表的方法相比，分析物的分离时间更短。分析柱为MZ Kromasil C18，5微米，250×4毫米，在室温下操作，背压值为230千克/平方厘米。流动相由甲醇-乙腈-0.1摩尔/升醋酸铵（45:15:40 v/v）组成，流速为1.0毫升/分钟。分别在激发波长325纳米和发射波长375纳米处进行荧光检测。水杨酸用作内标，浓度为0.5纳克/微升，奎宁的检测限为0.3纳克，线性范围上限为0.7纳克/微升，氯喹的线性范围上限为0.5纳克/微升。5分钟内完成分离。通过进行日内（n = 8）和日间校准（n = 8）对该方法进行了统计评估，结果发现该方法令人满意，具有高精度和高准确度。固相萃取从生物基质中提供了较高的相对萃取回收率：血清中奎宁的回收率为92.1%，氯喹为105.4%；尿液中奎宁的回收率为101.8%，氯喹为90.7%。
