离子色谱法测定血液等样品中的氟乙酸钠

Determination of Sodium Monofluoroacetate in Human Blood and Food Samples by Ion Chromatography

建立了离子色谱法测定血液样品中灭鼠剂氟乙酸钠的方法。在0 2mL血液样品中加入1mL纯水,然后用乙腈沉淀蛋白质,待蛋白沉降后取上清液经0 45μm过滤头过滤,滤液注进离子色谱仪进行氟乙酸钠的定性和定量分析。色谱条件:色谱柱为DionexIonPacAS11阴离子交换柱(250mm×4mmi.d.)及其相应的AG11保护柱(50mm×4mmi d ),流动相为2 0mmol/LNa2B4O7,微膜自再生阴离子抑制器,电导检测,25μL定量进样环。氟乙酸钠在0 10～10 0mg/L时,其峰面积与质量浓度呈良好的线性关系(r2=0.9978),实测溶液的检测限为0 05mg/L,血样中的检测限为2.5mg/L,平均加标回收率在85%以上。该法也可用于食物中氟乙酸钠的测定。

A method was developed for the determination of sodium monofluoroacetate in human blood by ion chromatography. The analysis was performed on a Dionex Ion Pac AS11 column (250 mm×4 mm i.d.) with an AG11 guard column (50 mm×4 mm i.d.). A conductivity detector, an SRS suppressor and a 25 μL sample loop were used. The eluent was 2.0 (mmol/L) Na_2B_4O_7 with a flow rate of 1.0 (mL/min). A blood sample of 0.2 mL was pipetted into a test tube followed by adding 1.0 mL of pure water. And then acetonitrile was used to dilute it to 3.0 mL. After the protein was settled down from the blood sample, the supernatant layer was filtered through a 0.45 μm filter before injected into the ion chromatographic system. Good linear relationship between the peak area and the concentration of sodium monofluoroacetate was found with correlation coefficient (r^2) of (0.997 8) within the range from 0.10 to 10.0 (mg/L). The detection limit for blood was 2.5 (mg/L). This method also can be used for the determination of sodium monofluoroacetate in food samples.