正相高效液相色谱法测定小鼠肝与血中伯氨喹和肝靶向药NGA－PQ的浓度

Determination of Primaquine and Hepatic Targeting Neoglycoalbumin- Primaquine in Whole Blood and Liver of Mouse by Normalphase High-performance Liquid Chromatography

建立了以紫外２５４ｎｍ波长检测的正相高效液相色谱法测定小鼠肝和血中伯氨喹（ＰＱ）和肝靶向ＰＱ（ＮＱＡ－ＰＱ）的浓度。填料为ＳｉＯ＿２，流动相为氯仿：甲醇：氨液（８６．８：１２．５：０．７，Ｖ／Ｖ／Ｖ），内标用６－甲氧基－８－（４－氨基丁酰胺基）－喹啉，方法回收率为１００．０９±３．４６，日内变异系数２．７％～６．１３％（ｎ＝５），日间变异系数为８．３０％～１３．５６％（ｎ＝９），磷酸伯氨喹和ＮＧＡ－ＰＱ以ＰＱ碱基计，最低检测浓度分别为２ｎｇ／ｍｌ和５０ｎｇ／ｍｌ全血或ｌｇ肝匀浆。内源性物质不干扰色谱测定。

We have developed a method to esti-mate primaquine(PQ)and hepatic targeting antimala-rial agent neoglycoalbumin-primaquine(NGA PQ)inwhole blood and Iiver of mice by sensitive and selectivehigh-performance Iiquid chromatography. The pri-maquine was extracted out with ether from the basifiedbiological samples in the PQ diphosphate group orfrom the samples which were acidic hydrolyzed thenbasified in NGA-PQ group.The extracts were evapo-rated under N_2 then dissolved in the mobile phass .A Iinear chain analogue of primaquine was used as the in-ternal standard.The samples were injected into thenormal phase silica column with chloroform:methanol:ammonia solution(86.8:12.5:0.7,V/V/V)as mobile phase and detected at 254nm. The aver-age recovery of the method was 100.09±3.46(x±s)%;the CV of within-day and between-day were 2.7%-6.13%(n=5)and 8.32%-13.56%(n=9)re-spectively;in PQ group and NGA-PQ group,the PQconcentrations ranged from 10-20 000 ng/ml blood orlg. Iiver rexpectively,and they all yielded a good Iinearrelationship with the peak height ratios. No endoge-neous interference was found in chromatograms of bio-logical samples.