论文部分内容阅读
目的建立高效液相色谱法测定工作场所空气中对甲苯磺酸的方法。方法利用浸渍超细玻璃纤维滤纸采集工作场所空气中气溶胶态以及蒸气态对甲苯磺酸,异丙醇-水洗脱,离子对高效液相色谱法测定。结果方法检出限1.0μg/ml、定量下限为3.3μg/ml。测量范围0μg/ml～1 000μg/ml,相关系数(R2)大于0.999,其回归方程斜率(Mean±SD)为0.4821±0.0112。精密度:每张滤膜含100μg、500μg、2 500μg对甲苯磺酸时,连续5 d 6次测定,其日内精密度(RSD)为1.9%～2.7%,日间精密度为2.3%～2.6%。实际样品加标回收率在91.6%～102.8%之间。超细玻璃纤维滤纸采集气溶胶态对甲苯磺酸的平均采样效率为95.7%、浸渍超细玻璃纤维滤纸采集蒸气态对甲苯磺酸的平均采样效率为95.2%。样品用异丙醇∶水(2∶98,V/V)洗脱,其洗脱效率大于97%。(浸渍)超细玻璃纤维滤纸采集对甲苯磺酸,在室温下至少可保存7 d。结论该方法具有较高的准确度、采样效率和解吸效率,较低的检出限,较好的精密度和稳定性,能满足了工作场所空气中对甲苯磺酸浓度的测定要求。
Objective To establish a method for the determination of p-toluenesulfonic acid in the air of workplace by high performance liquid chromatography. Methods The airborne aerosol in the workplace was collected by immersing superfine glass fiber filter paper, and the p - toluenesulfonic acid and isopropanol - water were used as the eluents in the workplace. The contents were determined by ion - pair high performance liquid chromatography. Results The detection limit was 1.0μg / ml and the limit of quantitation was 3.3μg / ml. The measurement range was 0μg / ml ~ 1 000μg / ml, the correlation coefficient (R2) was greater than 0.999, and the slope of regression equation was 0.4821 ± 0.0112. Precision: Each filter contained 100μg, 500μg and 2 500μg p-toluenesulfonic acid for 6 consecutive days, with the intra-day precision (RSD) of 1.9% -2.7% and the intraday precision of 2.3% -2.6 %. The actual sample spiked recoveries ranged from 91.6% to 102.8%. The average sampling efficiency of aerosol p-toluenesulfonic acid collected from ultrafine glass fiber filter was 95.7%. The average sampling efficiency of vapor-state p-toluenesulfonic acid collected from impregnated superfine glass fiber filter was 95.2%. Samples were eluted with isopropanol: water (2:98, V / V) with an elution efficiency greater than 97%. (Impregnated) superfine glass fiber filter paper p-toluenesulfonic acid collected at room temperature can be stored for at least 7 d. Conclusion The method has high accuracy, sampling efficiency and desorption efficiency, lower detection limit, better precision and stability, which can meet the determination of p-toluenesulfonic acid concentration in the air of the workplace.