从生物体液中分离舍曲林条件的建立

S. V. Baiurka, S. A. Karpushyna
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摘要

抗抑郁药物的毒理学意义正在稳步提高。开发有效的样品制备方法是抗抑郁药化学毒理学分析的热点问题。建立液液萃取法从血液和尿液中分离抗抑郁药舍曲林的条件。材料和方法。这些研究是用添加了舍曲林的模型血液和尿液样本进行的。在血液的研究中,通过添加10%的三氯乙酸溶液来预沉淀形成的血液元素。正己烷萃取纯化pH为1,氯仿萃取生物液pH为8。得到的提取物进一步进行薄层色谱纯化。采用紫外分光光度法测定洗脱液中舍曲林的含量。结果和讨论。舍曲林在甲醇- 25%氢氧化铵溶液(100:10.5)流动相中的Rf值为0.42±0.02。洗脱液的紫外光谱在268±2、275±2和283±2 nm处有最大吸收波长,与舍曲林标准溶液在0.1 mol /L盐酸乙醇溶液中的紫外光谱相匹配。在λmax 275 nm处,根据标定曲线y = 0,00216x - 0,03进行定量测定。所建立的方法可从尿液中分离出80.0±4.0%的舍曲林,从血清中分离出39.0±2.0%的舍曲林,从血清分离后的血液沉积物中分离出8.0±0.7%的抗抑郁药。确定了液液萃取法制备抗抑郁药舍曲林生物液样品的有效条件。所获得的结果对于创建一个算法的毒理学研究的生物样品,这种抗抑郁药的存在,在致命的药物中毒的情况下具有实际意义。
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Development of conditions for sertraline isolation from biological fluids
The toxicological significance of antidepressant drugs is steadily increasing. Development of the effective methods of the sample preparation is a topical issue of the chemical-toxicological analysis of antidepressants. Aim. To develop conditions for isolating the antidepressant sertraline from the blood and urine by the liquid-liquid extraction. Materials and methods. The studies were performed with model blood and urine samples spiked with sertraline. In the study of the blood, the formed blood elements were pre-precipitated by adding a 10 % solution of trichloroacetic acid. Extraction purification was performed with hexane at pH 1, and the drug was extracted from biological fluids with chloroform at pH 8. The extracts obtained were further subjected to the TLC purification. Determination of sertraline in eluates from chromatograms was performed by the UV spectrophotometric method. Results and discussion. The Rf value of sertraline in the mobile phase of methanol – 25 % ammonium hydroxide solution (100:10.5) was 0.42 ± 0.02. The UV spectra of the eluates from the chromatograms had absorption maxima at wavelengths of 268 ± 2, 275 ± 2 and 283 ± 2 nm and matched with the UV spectrum of a standard solution of sertraline in 0.1 mole/L ethanol solution of hydrochloric acid. The quantitative determination was performed at λmax 275 nm according to the equation of the calibration curve y = 0,00216x–0,03. The methods developed allowed to isolate 80.0 ± 4.0 % of sertraline from the urine, 39.0 ± 2.0 % from the blood serum, and additionally 8.0 ± 0.7 % of the antidepressant studiedfrom the blood sediment after its separation from the blood serum. Conclusions. The effective conditions for the sample preparation of biological fluids using the liquid-liquid extraction method for the antidepressant sertraline have been determined. The results obtained are of practical importance for creating an algorithm for the toxicological study of biological samples for the presence of this antidepressant in case of fatal drug intoxications.
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