摘要
目的：建立反相高效液相色谱-紫外光谱法快速检测食物中毒样品中的敌鼠钠盐的分析方法。方法：以ODS—C18色谱柱（150mm×4．6mm）为分离柱分离，以醋酸铵-乙腈为流动相，在波长286nm下，考察了醋酸铵缓冲溶液pH、浓度以及流动相不同体积比、总流速、柱温、不同提取溶剂等因素影响，建立了测定敌鼠钠盐的前处理和液相分析的最佳测定条件。结果：方法测定敌鼠钠盐的线性范围为0．050—10．0μg／ml，相关系数为0．9997。以3倍信噪比计算最低检测浓度为0．01μg／ml，最低检出量为0．1ng。样品加标回收率为86．9％～97．3％，相对标准偏差为2．3％-4．3％（n=3）。样品经乙腈提取过滤后直接进样，分离测定过程在10min之内完成。结论：本方法快速、灵敏、准确，满足食物中毒应急检测需要，及时为临床医师提供诊断、用药依据。
Objective： To establish a rapid method to determine diphacinone - Na in food poisoning samples by RP - HPLC. Methods：Diphacinone - Na was separated by a ODS - C18 column （ 150 mm ×4. 6 mm i. d, 4. 6 μm） and detected at the wavelength of 286 nm. The analytical conditions of RP - HPLC were optimized including the pH and concentration of ammonia acetate buffer solution, the ration and total flow rate of mobile phase, the temperature of column oven and extraction solvent etc. Results ：The linear range of diphacinone - Na was 0.05 -20. 0 μg/ml, and the correlation coefficient was 0. 9997. The recoveries were from 86. 9% to 97.3%. The relative standard deviations were between 2. 3% and 4. 3% （ n = 3 ）. Samples were extracted by acetonitrile directly. The seperation and detection were completed within 10 minutes. Conclusion： The method is simple, fast and accurate. It can answer for the requirements to determine diphacinone - Na in food poisoning accidents.
出处
《中国卫生检验杂志》
CAS
2007年第3期458-459,484,共3页
Chinese Journal of Health Laboratory Technology
