Citation:
SHI Ying, ZHANG Jing, LU Libin, SHAO Bing. Determination of triclosan and triclocarban in human nails by solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography,
;2013, 31(11): 1040-1045.
doi:
10.3724/SP.J.1123.2013.05032
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An analytical method was developed to simultaneously detect triclosan (TCS) and triclocarban (TCC) in human nails using solid phase extraction (SPE) with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Nail clippings were digested by sodium hydroxide, and then concentrated and purified with C18 cartridges. Chromatographic separation was performed on a Waters ACQUITYTM UPLC HSS T3 column (100 mm×2.1 mm, 1.8 μm) with gradient elution using methanol and water at a flow rate of 0.3 mL/min. The target compounds were determined by triple quadrupole mass spectrometer operated in the negative ion mode and quantified by isotopic-dilution technique. The satisfactory linearities (r2=0.999) was obtained over the ranges of 0.5-500.0 μg/kg for TCS and 0.1-100.0 μg/kg for TCC, with the limits of quantification (LOQs) of 2.0 μg/kg for TCS and 0.2 μg/kg for TCC. The average recoveries of the two target compounds (spiked at three concentration levels) ranged from 95.9% to 110.2%, with the relative standard deviations (RSDs) between 0.6% and 9.7% (n=6). This method can be applied in rapid detection of target contaminants in nails due to its high sensitivity, high recovery and good reproducibility. Sixty collected human nail samples were analyzed by means of the developed method. TCS and TCC were detected in all samples with content ranges of
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Keywords:
- solid phase extraction (SPE),
- ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),
- triclosan,
- triclocarban,
- nail
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