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目的建立高效液相色谱/二极管阵列检测法同时测定尿样中马尿酸、(邻,间,对)-甲基马尿酸含量的方法。方法以0.5 ml乙酸乙酯为萃取溶剂,样品用量0.5 ml,NaCl加入量75 mg,萃取时间3 min,以1000 r/min速度离心5 min,取0.4 ml萃取剂于具塞试管在低于70℃水浴中挥发至干,用1.0 ml流动相溶解残留物,分析条件:柱温35℃,流动相(甲醇:水:冰乙酸=30:70:0.1)波长235 nm,实现了4种代谢物的有效分离。结果在优化条件下,4种待测组分在20 mg/L~500 mg/L范围内呈线性,相关系数(r)均不低于0.9997,检出限(S/N=3)为21μg/L~200μg/L;样品的平均加标回收率为97%~104%,相对标准偏差(RSD)小于5%。结论该方法确定了最佳样品预处理条件,优化了色谱分离及检测条件,灵敏、准确,能够满足有害物质代谢产物的监测要求。
OBJECTIVE To establish a method for the simultaneous determination of hippuric acid (o-, m-, p-) hippuric acid in urine samples by high performance liquid chromatography / diode array detection. Methods With 0.5 ml ethyl acetate as extraction solvent, the amount of sample was 0.5 ml, the amount of NaCl was 75 mg, the extraction time was 3 min, centrifuged at 1000 r / min for 5 min, ℃ water bath to volatilize to dryness and dissolve the residue with 1.0 ml of mobile phase. The analysis conditions were: column temperature 35 ℃, mobile phase (methanol: water: glacial acetic acid = 30: 70: 0.1) Effective separation. Results Under the optimum conditions, the four analytes were linear in the range of 20 mg / L to 500 mg / L with the correlation coefficient (r) of no less than 0.9997 and the limit of detection (S / N = 3) of 21 μg / L ~ 200μg / L. The average recoveries of samples were 97% -104% with relative standard deviations (RSDs) less than 5%. Conclusion This method has determined the best sample pretreatment conditions, optimized chromatographic separation and detection conditions, sensitive and accurate, and can meet the monitoring requirements of metabolites of harmful substances.