UPLC-MS/MS用于女童尿液中6种酚类化合物的测定

Determination of Six Phenolic Compounds in Urine of Girls by UPLC-MS/MS

目的建立儿童尿样中6种酚类化合物的超高效液相色谱—串联质谱(UPLC-MS/MS)的测定方法。方法采用UPLC-MS/MS测定女童尿液中双酚A(BPA)、4-壬基酚(NP)、4-正辛基苯酚(OP)、4-庚基苯酚(HP)、4-戊基苯酚(NAP)和2-丙基苯酚(NPP)。尿液经酶解、液液萃取、氮吹至近干,甲醇定容后上机检测。结果6种化合物在(0.5~20)ng/mL浓度范围内线性关系良好,相关系数>0.999。检出限(LOD)在(0.16~0.30)ng/mL。在1、10和20 ng/mL添加水平下,回收率为88%~118%,相对标准偏差(RSD)为2.1%~8.9%。用此方法测定中枢性性早熟女童(病例组)与健康女童(对照组)的尿样,病例组中6种酚类化合物的检出率高于对照组。结论本方法适于儿童尿样中6种酚类化合物的测定。

Objective To established a method for determination of six phenolic compounds in the children’s urine by by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods UPLC-MS/MS was used to determine Bisphenol A(BPA), 4-nonylphenol(NP), 4-n-octylphenol(OP), 4-heptylphenol(HP), 4-pentylphenol(NAP), and 2-propylphenol(NPP) in the urine of girls. The urine was test after enzymatic hydrolysis, liquid-liquid extraction, nitrogen blowing to almost dryness, and diluting to volume with methanol. Results The six compounds had good linear relationship within the concentration range of(0.5-20)ng/mL, with correlation coefficients all above 0.999. The limit of detection(LOD) was(0.16-0.30)ng/mL. At spiking levels of 1, 10, and 20 ng/mL, the recoveries of samples were 88%-118%, and the relative standard deviations(RSD) were 2.1%-8.9%. Using this method to examine the urine samples of girls with central precocious puberty(case group) and healthy girls(control group), the detection rate of six phenolic compounds in the case group was higher than that in the control group. Conclusion The method is applicable to determination of six phenolic compounds in the children’s urine.