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Determination of the immunosuppressant mycophenolic acid in human serum by solid-phase microextraction coupled to liquid chromatography

机译:固相微萃取-液相色谱法测定人血清中的免疫抑制剂麦考酚酸

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摘要

A solid phase microextraction (SPME)–HPLC–UV method for the determination of the immunosuppressant mycophenolic acid (MPA) in human serum samples was developed for the first time. The procedure, that employed a carbowax/templated resin (Carbowax/TPR-100) as fiber coating, required a very simple sample pretreatment, an isocratic elution, and provides an highly selective extraction. The linear range was 0.2–100 μg ml~(-1). Recovery was practically unchanged (63±4%) passing from 0.2 to 100 μg ml~(-1) level. Within-day and between-days coefficient of variation ranged from 5.9 to 6.5% and from 8.8 to 9.2%, respectively. A detection limit of 0.05 μg ml~(-10 was estimated in spiked serum. The method was successfully applied to the determination of MPA in serum of a patient under mycophenolate mophetil ester (MMF) therapy, as demonstrated by the relevant concentration-time profiles.
机译:首次开发了一种固相微萃取(SPME)-HPLC-UV方法测定人血清样品中的免疫抑制剂麦考酚酸(MPA)。该方法使用碳纤维/模板树脂(Carbowax / TPR-100)作为纤维涂层,需要非常简单的样品预处理,等度洗脱并提供高度选择性的提取。线性范围为0.2–100μgml〜(-1)。回收率从0.2到100μgml〜(-1)几乎没有变化(63±4%)。日内和日间变异系数分别为5.9%至6.5%和8.8%至9.2%。相关浓度-时间曲线证明,该方法在加标血清中的检出限估计为0.05μgml〜(-10),该方法已成功地用于霉酚酸酯,甲基苯丙酸酯(MMF)治疗下患者血清中MPA的测定。

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