高效液相色谱法对工作场所空气中β-萘酚的测定

Determination ofβ-naphthol in the air of workplace by high performance liquid chromatography

目的以现行方法为基础优化工作场所空气中β-萘酚的高效液相色谱测定方法,从而高效、快速、准确地检测工作场所空气中的β-萘酚。方法本研究采用微孔滤膜采集工作场所空气中的β-萘酚,采样后的滤膜样品放入试管中加入5.0 ml甲醇,试管中洗脱30 min,以甲醇-水为流动相进行梯度洗脱,用高效液相色谱-紫外检测器进行测定,标准曲线法定量,分别测定方法检出限、最低检出浓度、方法相对标准偏差(RSD)、平均洗脱效率等指标。结果β-萘酚在质量浓度为1.0~10.0μg/ml时相关性良好,相关系数均≥0.9992;方法检出限为0.002μg/ml,最低检出浓度为0.001 mg/m^(3)(以采集75 L空气样品计算);方法的批内RSD为1.19%~1.67%,批间RSD为1.44%~2.33%,平均洗脱效率为92.1%~95.2%;样品在室温下可保存7 d。结论高效液相色谱法样品使用量少、分离效能高、操作简单、节约时间、结果准确可靠,适用于工作场所空气中β-萘酚水平的测定。

Objective Based on the current method,to optimize the determination method ofβ-naphthol in the air of workplace by high performance liquid chromatography(HPLC),so as to detectβ-naphthol in the air of workplace efficiently,rapidly and accurately.Methods In this study,β-naphthol was collected in the air of workplace using microporous membrane.After sampling,5.0 ml methanol was added into the test tube for elution for 30 mintues,by using methanol-water as the mobile phase for gradient elution.Using HPLC-UV detector for determination and standard curve for quantification,indicators such as method detection limit,minimum detectable concentration,method relative standard deviation(RSD),and average elution efficiency were determined respectively.Results The correlation was good when the mass concentration ofβ-naphthol was 1.0-10.0μg/ml,with the correlation coefficients≥0.9992;the method detection limits was 0.002μg/ml,and the minimum detectable concentrations was 0.001 mg/m^(3)(calculated by collecting 75 L air sample).The within-run RSD was 1.19%-1.67%,and the between-run RSD was 1.44%-2.33%,the average elution efficiency of the method was 92.1%-95.2%.The samples could be stored at room temperature for 7 days.Conclusion HPLC boasted less sample usage,high separation efficiency,simple operation,time saving,accurate and reliable results.It was applicable to the determination ofβ-naphthol level in the air of workplace.