One-step sample processing method for the determination of perchlorate in human urine, whole blood and breast milk using liquid chromatography tandem mass spectrometry.

ABSTRACT

A one-step sample processing was developed to determine the levels of perchlorate in human urine, whole blood and breast milk by using liquid chromatography tandem mass spectrometry (LC-MS/MS). Athena C18-WP column was used to separate and analyze perchlorate. Perchlorate and isotope-labeled perchlorate (Cl18O4-) internal standards were spiked in the sample matrix through vortex mixing, centrifugation, and filtration. The filtrate was collected and subjected to LC analysis. The developed method was validated for its reproducibility, linearity, trueness, and recovery. Satisfactory recovery of perchlorate ranged from 81% to 117% with intraday relative standard deviations (RSDs) (n = 3) and inter-day RSDs (n = 9) of 5-18% and of 5-16%, respectively. Good linearity (R2 ≥ 0.99) was observed. Limits of detection and quantification for perchlorate ranged from 0.06 µg/L to 0.3 µg/L and from 0.2 µg/L to 1 µg/L, respectively. Perchlorate concentrations were found in human urine (n = 38) and whole blood (n = 8) samples with the range of 6.5-288.6 µg/L and 0.3-2.8 µg/L, respectively. These results indicate the applicability of our developed method in determining perchlorate level in real samples. Moreover, this method is also highly reliable, sensitive and selective in detecting perchlorate in human urine, whole blood and breast milk samples and may be applicable to other matrixes i.e. saliva, serum, plasma, milk powder and dairy milk.