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[采用正相高效液相色谱法测定小鼠全血和肝脏中伯氨喹及肝靶向性新糖白蛋白-伯氨喹]

[Determination of primaquine and hepatic targeting neoglycoalbumin-primaquine in whole blood and liver of mouse by normalphase high-performance liquid chromatography].

作者信息

Li T, Pang Q, Jia Y, Wang P, Ma T, Meng J, Zhao S

出版信息

Hua Xi Yi Ke Da Xue Xue Bao. 1995 Mar;26(1):109-12.

PMID:7657325
Abstract

We have developed a method to estimate primaquine (PQ) and hepatic targeting antimalarial agent neoglycoalbumin-primaquine (NGA PQ) in whole blood and liver of mice by sensitive and selective high-performance liquid chromatography. The primaquine was extracted out with ether from the basified biological samples in the PQ diphosphate group or from the samples which were acidic hydrolyzed then basified in NGA-PQ group. The extracts were evaporated under N2 then dissolved in the mobile phase. A linear chain analogue of primaquine was used as the internal standard. The samples were injected into the normal phase silica column with chloroform: methanol:ammonia solution (86.8:12.5:0.7,V/V/V) as mobile phase and detected at 254 nm. The average recovery of the method was 100.09 +/- 3.46 (mean +/- s)%; the CV of within-day and between-day were 2.7%-6.13% (n = 5) and 8.32%-13.56% (n = 9) respectively; in PQ group and NGA-PQ group, the PQ concentrations ranged from 10-20,000 ng/ml blood or 1g. liver respectively, and they all yielded a good linear relationship with the peak height ratios. No endogeneous interference was found in chromatograms of biological samples.

摘要

我们开发了一种通过灵敏且具选择性的高效液相色谱法来测定小鼠全血和肝脏中伯氨喹(PQ)以及肝靶向抗疟剂新糖白蛋白 - 伯氨喹(NGA - PQ)的方法。在二磷酸伯氨喹组中,用乙醚从碱化的生物样品中提取伯氨喹;在NGA - PQ组中,从经酸性水解后再碱化的样品中提取伯氨喹。提取物在氮气下蒸发,然后溶解于流动相中。使用伯氨喹的线性链类似物作为内标。将样品注入以氯仿∶甲醇∶氨溶液(86.8∶12.5∶0.7,V/V/V)为流动相的正相硅胶柱,并在254 nm波长处进行检测。该方法的平均回收率为100.09±3.46(均值±标准差)%;日内变异系数和日间变异系数分别为2.7% - 6.13%(n = 5)和8.32% - 13.56%(n = 9);在PQ组和NGA - PQ组中,PQ在血液中的浓度范围分别为10 - 20,000 ng/ml,在肝脏中的浓度范围分别为1μg/g,且它们与峰高比均呈现良好的线性关系。在生物样品的色谱图中未发现内源性干扰。

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