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Determination of parabens in human urine by liquid chromatography coupled with electrospray ionization tandem mass spectrometry

机译:液相色谱-电喷雾串联质谱法测定人尿中对羟基苯甲酸酯

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A simple and sensitive method was developed for the simultaneous determination of methyl, ethyl, n-propyl, n-butyl, and benzyl parabens in human urine by liquid chromatography coupled with electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS). Enzymatic hydrolysis conditions were optimized to deconjugate the urinary parabens, glucuronide and sulfate conjugates. Solid phase extraction (SPE) was then used for sample clean-up. LC-ESI-MS/MS conditions for sample analysis were also optimized to achieve the maximal sensitivity and accuracy. Parabens were finally separated on a C8 reversed phase column. Correlation coefficients (R~2) and recoveries ranged from 0.998 to 0.999 and 80.6% to 95.6%, respectively, and intra-day and inter-day precisions (relative standard deviation, RSD) were within 1.2-4.5% and 2.2-7.1%, respectively. Limits of detection (LODs) for methyl, ethyl, n-propyl, n-butyl, and benzyl parabens were 3, 3, 3, 3, and 1 pg, respectively. The optimized method was successfully used to determine parabens in urine samples from school students in Southern China.
机译:通过液相色谱-电喷雾串联质谱法(LC-ESI-MS / MS),开发了一种简单灵敏的方法,可同时测定人尿中的对羟基苯甲酸甲酯,乙基,正丙基,正丁基,正丁基和对羟基苯甲酸苄酯。优化了酶水解条件以解离尿对羟基苯甲酸酯,葡糖醛酸苷和硫酸盐结合物。然后将固相萃取(SPE)用于样品净化。还优化了用于样品分析的LC-ESI-MS / MS条件,以实现最大的灵敏度和准确性。最终将对羟基苯甲酸酯在C8反相柱上分离。相关系数(R〜2)和回收率分别为0.998至0.999和80.6%至95.6%,并且日内和日间精度(相对标准偏差,RSD)在1.2-4.5%和2.2-7.1%之内, 分别。甲基,乙基,正丙基,正丁基,对羟基苯甲酸苄酯的检出限(LOD)分别为3、3、3、3和1 pg。该优化方法已成功用于测定华南在校学生尿液样本中的对羟基苯甲酸酯。

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