尿中苯乙醇酸和苯乙醛酸测定的免试剂离子色谱法

Determination of mandelic acid and phenylglyoxylic acid in urine by reagent-free ion chromatography

目的 建立尿中苯乙醇酸（MA）和苯乙醛酸（PGA）测定的免试剂离子色谱法.方法 利用离子色谱仪,选用AS19阴离子分析柱,10～35 mmol/L KOH梯度淋洗,流速为1.00 ml/min,紫外检测波长：MA 225 nm,PGA 254 nm.样品用纯水10倍稀释后,经银柱去除高浓度氯离子,0.2 μm滤膜过滤后进样.结果 MA和PGA的加标回收率为96.5％～99.3％,相对标准偏差均小于5.0％,在1.0～100.0 mg/L范围均呈现良好的线性关系,回归系数大于0.999 5.MA和PGA检出限分别为0.02和0.05 mg/L;最低检出浓度分别为0.2和0.5 mg/L（取样量为5.0 ml,纯水定容至50.0 ml,进样量为300μl）.结论 该方法快速简单,灵敏度高,选择性强,可应用于苯乙烯工作场所工人尿中MA和PGA的检测.

Objective To develop a method for determination of mandelic acid （MA） and phenylglyoxylic acid （PGA） in urine by reagent-free ion chromatography.Methods Ion chromatography was performed on an AS19 column with a gradient elution solution containing 10～35 mmol/L KOH at a flow rate of 1.00 ml/min,and MA and PGA were detected at ultraviolet wavelengths of 225 nm and 254 nm,respectively.The samples were diluted 10 times with purified water,then purified on a silver column to remove high concentrations of chloride ion,and injected after being filtered through a 0.2-μm filter membrane.Results The recoveries of standard addition of MA and PGA were 96.5% and 99.3%,respectively,with both relative standard deviations less than 5.0%.Good linear relationships were noted in the range of 1.0～100.0 mg/L for both MA and PGA （r 〉0.9995）.The detection limits of MA and PGA were 0.02 mg/L and 0.05 mg/L,respectively;the minimum detectable concentrations of MA and PGA were 0.2 mg/L and 0.5 mg/L （when the sampling amount was 5.0 ml and diluted to 50.0 ml with water,and the injection volume was 300 μL）.Conclusions This method is fast,convenient,and highly sensitive and selective.It can be used for the analysis of MA and PGA in the urine of styreneexposed workers.