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目的建立血液等生物样品中氟乙酸钠的离子色谱测定方法。方法采用Ionpac誖AS9-HC阴离子交换柱和AG9-HC保护柱,流动相为9.0 mmol/L碳酸钠溶液。样品中的蛋白质经乙腈沉淀,离心,过C18柱,经0.22μm过滤头过滤,直接进样测定。结果该方法的线性范围为0.1~10.0 mg/L,相关系数为0.999 8(n=6),相对标准差(RSD)为6.7%～0.26%。最低检出限为0.01 mg/L,定量检出限为0.1 mg/kg。样品回收率为93.8%~103.6%。结论该方法操作简单,快速,准确,分离效果好,可与常见共存阴离子同时分析,灵敏度高,重现性好,可满足对血样、尿样、食品及饵料样中氟乙酸钠的测定。
Objective To establish a method for the determination of sodium fluoroacetate in blood and other biological samples by ion chromatography. Methods Ionpac paradox AS9-HC anion exchange column and AG9-HC guard column with a mobile phase of 9.0 mmol / L sodium carbonate solution. The protein in the sample was precipitated by acetonitrile, centrifuged, filtered through a 0.18 μm filter and directly injected into the C18 column. Results The linear range of this method was 0.1-10.0 mg / L with a correlation coefficient of 0.999 8 (n = 6) and a relative standard deviation (RSD) of 6.7% -0.26%. The minimum detectable limit is 0.01 mg / L and the limit of quantification is 0.1 mg / kg. The recoveries of samples ranged from 93.8% to 103.6%. Conclusion The method is simple, rapid and accurate, and has good separation effect. It can be simultaneously analyzed with common coexisting anions and has high sensitivity and good reproducibility. It can meet the determination of sodium fluoroacetate in blood samples, urine samples, food and feed samples.