Optimization of the detection method for urine S-phenylmercapturic acid via modified performance liquid chromatography-mass spectrometry
- Author:
CUI Shi wei ZHOU Xiao ying XING Cai hong YAN Hui fang
- Publication Type:Journal Article
- Keywords:
S phenylmercapturic acid Solid phase extraction Isotope Internal standard Performance liquid
- From:
China Occupational Medicine
2022;49(06):692-696
- CountryChina
- Language:Chinese
-
Abstract:
Objective -
To optimize the extraction and quantification methods for the determination of S phenylmercapturic acid
- Methods
(SPMA) in urine with performance liquid chromatography mass spectrometry. The urine was hydrolyzed with 50.0%
sulfuric acid. The hydrolysate was purified by solid phase extraction column. Purified samples were separated by C18
chromatographic column and detected by tandem mass spectrometry. The isotope labeled SPMA was used as the internal
Results -
standard. The internal standard curve was used for quantification. The linear range of SPMA was 0.50 50.00 μg/L with
the correlation coefficient of 0.999 8. The detection limit and the lower limit of quantification were 0.05 and 0.17 μg/L,
- - - -
respectively. The recovery rate was 97.0% 102.0%. The within run and between run relative standard deviation were 0.6% 1.0%
-
and 1.7% 6.5%, respectively. The mass concentration of urinary SPMA in the occupational benzene exposure group was
- vs P
higher than the non occupational benzene exposure group by this method (median: 2.81 0.28 μg/g creatinine, <0.05).
Conclusion
Compared to the national standard method, this optimized method of solid phase extraction and internal standard
for quantification eliminates the matrix effect. This method is accurate and precise, and is suitable for the determination of SPMA
acid in urine.
