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Issue 9, 2011
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Ultra-performance liquid chromatographic assay coupled with two-dimensional separation for spectrometric determination of urinary S-phenylmercapturic acid

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Abstract

A gradient ultra-performance liquid chromatographic (UPLC) assay coupled with the two dimensional separation and diode array detection method was developed to determine S-phenylmercapturic acid (SPMA), a specific urinary metabolite of benzene. Gradient separation was performed on two C18 core–shell columns (2.6 and 1.7 μm, 50 × 2.1 mm i.d.) maintained at 40 and 20 °C. Among various solvents evaluated, dichloromethane which offered >85% recovery rates of both SPMA and D-benzylmercapturic acid (internal standard) was used for extraction. The yield of free-SPMA was maximized by hydrolyzing 200 μL of urine with 20 μL of 6 M HCl prior to dichloromethane extraction. The limit of detection was 1 μg L−1(s/n = 5) and the limit of quantification was 2 μg L−1. Using our method, a correlation of 0.99 was obtained with 10 specimens (range, 1.7 to 182 μg L−1) from the German External Quality Assessment Scheme. Among the 75 non-occupational exposure individuals, 61 (81%) had SPMA levels below the LOQ. Among the 26 male petroleum workers, 5 who were exposed to <0.04 ppm of benzene were found to have SPMA levels below the LOQ. The geometric means obtained from the other 15 non-smokers and 6 smokers who were exposed to <0.5 ppm of benzene were 5.05 and 6.65 μg g−1creatinine, respectively. The proposed method can be useful for occupational benzene exposure surveillance.

Graphical abstract: Ultra-performance liquid chromatographic assay coupled with two-dimensional separation for spectrometric determination of urinary S-phenylmercapturic acid

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Publication details

The article was received on 21 Feb 2011, accepted on 05 Jun 2011 and first published on 27 Jul 2011


Article type: Paper
DOI: 10.1039/C1AY05089C
Anal. Methods, 2011,3, 2025-2031

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    Ultra-performance liquid chromatographic assay coupled with two-dimensional separation for spectrometric determination of urinary S-phenylmercapturic acid

    B. L. Lee, H. Y. Ong, S. E. Chia and C. N. Ong, Anal. Methods, 2011, 3, 2025
    DOI: 10.1039/C1AY05089C

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