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引用次数: 0
摘要
本研究成功建立了一种中空纤维液相微萃取(HF-LPME) -高效液相色谱(HPLC)联用法测定尿和血浆样品中微量洛伐他汀的方法。将洛伐他汀从15 mL pH为2的酸性样品溶液中提取到浸渍在中空纤维孔隙中的有机提取溶剂(正辛醇)中,然后再将其提取到中空纤维管腔中的酸化水溶液中。提取后,将受体相10µL注入高效液相色谱系统。为了获得较高的萃取效率,研究并优化了影响HF-LPME的参数,包括样品和萃取剂的pH、有机相类型、离子强度、搅拌速率、萃取时间和温度。在优化条件下(溶剂为1-辛醇,pH = 2, 45℃,750rpm搅拌45 min),相对回收率为85.2 - 97%,表明该方法具有分析分析被分析物浓度的能力。该技术对水、尿和血浆的预富集因子分别为199、185和170。获得了较好的精密度值(相对标准分割≤10.5%)。结果表明,HF-LPME方法具有良好的清除能力和较高的富集系数,可作为一种简便、灵敏的生物样品中药物监测方法。
Hollow fiber-based liquid-phase microextraction and HPLC-UV determination of lovastatin in biological fluids
In this study, a hollow fiber liquid-phase microextraction (HF-LPME) method coupled with high-performance liquid chromatography (HPLC) was successfully developed for the determination of trace levels of lovastatin in urine and plasma samples. Lovastatin was extracted from 15 mL of the acidic sample solution with a pH of 2 into an organic extracting solvent (n-octanol) impregnated in the pores of a hollow fiber and then back extracted into an acidified aqueous solution in the lumen of the hollow fiber. After extraction, 10 µL of the acceptor phase was injected into HPLC system. To obtain high extraction efficiency, the parameters affecting the HF-LPME, including pH of the sample and extractant phases, type of organic phase, ionic strength, stirring rate, extraction time, and temperature, were studied and optimized. Under the optimized conditions (solvent 1-octanol, pH = 2, 45 min stirring at 45°C with 750rpm), the relative recovery percentage was 85.2–97, which shows the capability of the method to analyze the analyte concentration. This technique provided preconcentration factor 199, 185, and 170 for water, urine, and plasma, respectively. Good precisions values (with relative standard division ≤ 10.5%) were obtained. The results indicated that the HF-LPME method has an excellent cleanup capacity and a high preconcentration factor and could serve as a simple and sensitive method for monitoring the drug in biological samples.
期刊介绍:
The Journal of Reports in Pharmaceutical Sciences(JRPS) is a biannually peer-reviewed multi-disciplinary pharmaceutical publication to serve as a means for scientific information exchange in the international pharmaceutical forum. It accepts novel findings that contribute to advancement of scientific knowledge in pharmaceutical fields that not published or under consideration for publication anywhere else for publication in JRPS as original research article. all aspects of pharmaceutical sciences consist of medicinal chemistry, molecular modeling, drug design, pharmaceutics, biopharmacy, pharmaceutical nanotechnology, pharmacognosy, natural products, pharmaceutical biotechnology, pharmacology, toxicology and clinical pharmacy.