高效液相色谱法测定工作场所空气中对甲苯磺酸  

Measurement of P-Toluenesulfonic Acid in Workplace Air by HPLC

作　　者：杜洪凤[1] 游钒[1] 沈月华[1] 汪良枢[1] 

机构地区：[1]四川省疾病预防控制中心,成都61004

出　　处：《预防医学情报杂志》2012年第9期751-757,共7页Journal of Preventive Medicine Information

摘　　要：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 measuring p - toluenesulfonic acid in workplace air by high performance liquid chromatography （HPLC）. Methods p - toluenesulfonic acid in vapor and aerosol in workplace air was sampled using impregnated ultra -fine glass fiber filter paper, extracted with isopropanol in water and measured by ion pair high performance liquid chromatography. Results The accuracy of detection was 1. 0μg/ mL and the limit of quantification was 3.3 μg/L with the measuring range from 0μg/mL to 1 000 μg/mL. The correlation coefficient （ R2） was greater than 0. 999 and the slope of the regression equation （Mean ± SD） was 0. 482 1 ±0. 011 2. Filter paper containing 100 μg, 500 μg or 2 500 μg of p -toluenesulfonic acid was analyzed 6 times for 5 consecutive days,. Its intra - day precision （RSD） was in the range of 1.9% to 2. 7% and the inter - day precision （RSD） was within the range of 2. 3% to 2.6%. The recovery of spiked samples was within the range of 91.6% to 102.8%. The mean p - toluenesulfonic acid aerosol sampling efficiency of ultra - fine glass fiber filter paper was 95.7%, and the mean p - toluenesulfonic acid vapor sampling efficiency of impregnated ultra -fine glass fiber filter paper was 95.2%. Samples were extracted with 2% （V/V） isopro-panol in water and the extraction efficiency was greater than 97.4%. After sampling p - toluenesulfonic acid, the （impregnated） ultra -fine glass fiber filter paper could be stored at room temperature for at least 7 days.Conclusion This method has high accuracy, sampling and extraction efficiency, low detection limit, good pre- cision and stability. It can be used for determination of p - toluenesulfonic acid in workplace air.

关 键 词：高效液相色谱 测定 工作场所空气 对甲苯磺酸 

分 类 号：R657.72[医药卫生—外科学]