工作场所空气中DBP和DOP高效液相色谱测定法的改进  

Improvement of HPLC determination method of DBP and DOP in workplace air

作　　者：王敏 宋为丽 江金凤 

机构地区：[1]湖北省武汉市职业病防治院,430015

出　　处：《职业与健康》2015年第17期2349-2351,共3页Occupation and Health

摘　　要：目的对国标方法进行方法学技术指标验证,以保证工作场所空气中邻苯二甲酸二丁酯（DBP）和邻苯二甲酸二辛酯（DOP）的高效液相色谱法测定结果的准确、可靠。方法对国标方法的仪器操作参考条件、标准曲线的线性、检出限、精密度、加标回收率技术指标按照GBZ/T 210.4-2008《工作场所空气中化学物质测定方法》进行验证。结果优化了操作条件,改变了流动相的比例,采用梯度洗脱方法,使硅胶管中原本与DBP不能分离而干扰其测定的杂质峰完全分离。标准曲线在0.0~10.13μg/ml范围,DBP和DOP的相关系数均为r=1.000,回归方程分别为Y=2.28×104X-1.57×103、Y=1.45×104X-1.03×103。方法检出限分别为0.012μg/ml、0.234μg/ml,最低检出浓度分别为0.008、0.156 mg/m3（以采集3 L空气计算）,高、低浓度的精密度DBP为4.1%、1.7%,DOP 2.5%、3.3%,解吸效率分别为91.79%和92.19%。结论工作场所空气中DBP和DOP的高效液相色谱测定法,按照标准的色谱条件,硅胶管中的杂质峰与DBP不能分离,严重影响了测定结果的准确性,经过改进后,各项技术指标均满足规范要求。方法灵敏、准确、可靠,适用于工作场所空气中DBP和DOP的测定。[Objective]To verify the national standard method in methodology,so as to ensure the accuracy and reliability of the results of determining DBP and DOP in workplace air by HPLC.[Methods]The instrument operation reference condition,linearity of standard curve,detection limit,precision,and recovery rate were verified according to GBZ/T 210.4-2008 ＂Method for Determination of Chemical Substances in Workplace Air＂.[Results]The new method optimized operating conditions,changed the proportion of mobile phase,adopted gradient elution,and isolated the impurity peak from DBP in silicone tube. The standard curve ranged between 0.0-10.13 μg/ml,the correlation coefficient r of DBP and DOP was both 1.000,the regression equation was Y=2.28×104X-1.57×103,Y=1.45×104X-1.03×103,respectively. And the detection limit and minimum detectable concentration was 0.012 μg/ml and 0.234 μg/ml,0.008 mg/m3 and 0.156 mg/m3（3L air）,respectively. The precision of DBP of high and low intensity was 4.1% and 1.7%,that of DOP was 2.5% and 3.3%,respectively. The desorption efficiency of DBP and DOP was91.79% and 92.19%,respectively.[Conclusion]The standard HPLC can not isolate DBP from impurity peak in determination of DBP and DOP in workplace air. After improvement,all indicators meet the requirements. This method is sensitive,accurate and reliable,and suitable for determination of DBP and DOP in workplace air.

关 键 词：邻苯二甲酸二丁酯 邻苯二甲酸二辛酯 工作场所空气 高效液相色谱 

分 类 号：R134.4[医药卫生—劳动卫生]