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Simultaneous derivatization and extraction of free cyanide in biological samples with home-made hollow fiber-protected headspace liquid-phase microextraction followed by capillary electrophoresis with UV detection by Liang Meng; Xin Liu; Bin Wang; Guijun Shen; Zhengqiao Wang; Ming Guo is a Chemistry article available to read on EtoBox.

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A new method is reported for the simultaneous derivatization and extraction of free cyanide in biological samples using home-made hollow fiber-protected headspace liquid-phase microextraction (HF-HS-LPME) followed by capillary electrophoresis (CE) determination. The acceptor phase containing Ni(II)-NH(3) (as derivatization agent), sodium carbonate and ammonium pyromellitate (as internal standard) is held within a hollow fiber membrane, affixed to a syringe needle and immersed in the headspace of sample container. The extracted cyanide from the neutral samples forms a stable Ni(CN)(4)(2-) complex which is determined by CE. Parameters affecting extraction efficiency were investigated and optimized. For optimum peak shapes, the capillary was coated with cetyltrimethylammonium bromide (CTAB). The calibration curve was linear for concentrations of CN(-) in the range from 0.1 to 20 micromol L(-1) (R(2)=0.9987). The LOD (S/N=3) was estimated to be 0.01 micromol L(-1) of CN(-) concentration. Such a detection sensitivity is high enough for free cyanide determination in common environmental and biological samples. Excellent repeatability of the extraction (RSD < or = 5.6%, n=5) was achieved.

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Author

Liang Meng; Xin Liu; Bin Wang; Guijun Shen; Zhengqiao Wang; Ming Guo

Publisher

Elsevier Science; Elsevier ; Elsevier BV (ISSN 1873-376X)

Published

2009

Language

EN

Field

Chemistry (Physical Sciences)