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目的建立测定人尿中游离型双酚A型与双酚F型二缩甘油醚(BADGE,BFDGE)及其水解衍生物浓度的同位素内标-液液萃取-高效液相色谱串联质谱(HPLC)测定法。方法采用不同萃取剂和不同规格固相萃取柱进行前处理,以含乙酸铵或甲酸的甲醇和水为流动相,以梯度洗脱方式用C18色谱柱对目标化合物进行分离。以正离子喷雾模式电离,多反应离子监测方式进行定性及定量检测。结果该方法检测BADGE、BFDGE和2种衍生物在0.25~50 ng/ml范围内满足线性要求(r=0.999)。以D6-BADGE作为内标物质,液液萃取法对4种目标化合物3个浓度水平的加标回收率均在80%~120%,最低检出限为0.08~0.15 ng/ml,定量限为0.25~0.50 ng/ml,日内和日间RSD<10%。结论该方法对人尿中BADGE、BFDGE及其水解代谢产物的测定具有较高的灵敏度和精确性,可满足尿液样本中痕量BFDGE的检测需要;实际样本检测表明双酚型二缩甘油醚类物质可能对我国人群存在较广泛的暴露。
OBJECTIVE To establish an isotope internal standard-liquid-liquid extraction-high performance liquid chromatography tandem mass spectrometry (HPLC) method for the determination of the concentrations of free bisphenol A and bisphenol F diglycidyl ethers (BADGE, BFDGE) and their hydrolyzed derivatives in human urine Assay. Methods Pretreatment with different extractants and different solid phase extraction columns was performed on a C18 column with gradient elution of methanol and water containing ammonium acetate or formic acid as the mobile phase. Ionization with positive ion spray mode, multiple reactive ion monitoring methods for qualitative and quantitative detection. Results The linearity (r = 0.999) of BADGE, BFDGE and two derivatives was detected by this method in the range of 0.25-50 ng / ml. With D6-BADGE as internal standard, the spiked recoveries of three target compounds were 80% -120% by liquid-liquid extraction with the detection limit of 0.08-0.15 ng / ml. The limit of quantification 0.25 ~ 0.50 ng / ml, intra-day and inter-day RSD <10%. Conclusion This method has high sensitivity and accuracy for the determination of BADGE, BFDGE and its metabolites in urine, which can meet the need of detection of trace BFDGE in urine samples. The actual samples show that bisphenol-type diglycidyl ether Substances may have a broader exposure to our population.