Determination of 10 metabolites of organophosphate flame retardants in human urine by liquid-liquid extraction coupled with UPLC-MS-MS
Objective To establish an analytical method for the detection oi 10 common metabolites oforganophosphate flame retardants(mOPFRs)in human urine by using liquid-liquid extraction and ultra-high-performance liquid chromatography tandem with mass spectrometry(UPLC-MS/MS).Methods Urine samples were enzymatically digested,and the solution pH was adjusted.Sodium chloride salting-out was employed,with acetonitrile and ethyl acetate as extractants to isolate the target compounds.The gradient elution mode was applied in chromatographic separation and the samples were detected by UPLC-MS/MS.Quantitative analysis of target compounds was achieved under optimized mass spectrometry conditions.Results The linear range of the instrumental method was 0.2 to 10 μg/L,with regression coefficients ranging from 0.994 to 0.999.The method detection limits were determined to be in the range of 0.004 to 0.066 μg/L,and the quantification limits were in the range of 0.014 to 0.221 μg/L.The spiked recovery rates ranged from 74.6％to 127.2％.Bio-monitoring of urine samples from the Zengcheng district,Guangzhou,revealed the presence of all 10 mOPFRs.However,four mOPFRs exhibited relatively low detection rates,while the detection rates of the remaining six metabolites were all above 60％.Stratified analysis by gender indicated a significantly higher concentration of BCEP in male urine compared to female urine,while there was no statistically significant difference in the concentration of total mOPFRs results between genders.Conclusion The method was reliable,sensitive and suitable for the determination of different mOPFRs in human urine samples.
万方数据
维普
