Citation: YANG Hua-Mei, HANG Li, YANG Jian-Guo, ZHANG Xue-Mei, HUANG Wei-Hong, LI Chen, JIANG Xiao-Li. Ultra Liquid Chromatography-Tandem Mass Spectrometry with Dansyl Chloride Pre-column Derivatization[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(3): 462-467. doi: 10.11895/j.issn.0253-3820.150764 shu

Ultra Liquid Chromatography-Tandem Mass Spectrometry with Dansyl Chloride Pre-column Derivatization

1.
Taizhou Center for Disease Control and Prevention, Taizhou 225300, China

Corresponding author: YANG Hua-Mei,
Received Date: 28 September 2015
Available Online: 7 December 2015

A method was developed for the quantification of cyclohexylamine in human urine samples by ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) with pre-column derivatization. After the refrigerated centrifugation of urine samples, cyclohexylamine in supernatant was derived with dansyl chloride and then its derivant was purified with solid phase extraction (SPE). The target compounds were separated on a Waters ACQUITY CSHTM C₁₈ column (50 mm×2.1 mm, 1.7 μm) with the gradient elution of methanol and water (containing 0.002 mol/L ammonium acetate) and were determined in electrospray positive ionization (ESI⁺) and multiple reaction monitoring (MRM) modes. The linear range was 2.5-200 μg/L for cyclohexylamine with the correlation coefficient more than 0.999. The recovery ranged from 98.7% to 102.3%, with the relative standard deviations (RSDs) of 3.1%-5.2%. The limit of detection (LOD) and the limit of quantitation (LOQ) were 1 μg/L and 3 μg/L. The results indicated that the method was accurate and reliable, and suitable for the detection of cyclohexylamine in urine samples. The urine samples of 200 primary school students were analyzed by this method and the positive rate of cyclohexylamine was 34.5%.
- Cyclohexylamine,
- Dansyl chloride,
- Derivatization,
- Solid phase extraction,
- Human urine samples,
- Ultra liquid chromatography-tandem mass spectrometry
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沈阳化工大学材料科学与工程学院沈阳 110142