Tags

Type your tag names separated by a space and hit enter

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.
J Chromatogr B Analyt Technol Biomed Life Sci. 2009 Nov 01; 877(29):3645-51.JC

Abstract

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. The feasibility of this method was demonstrated by analyzing human urine and saliva samples with spiked recoveries in the range of 92-103.4%. This work provided an efficient alternative to the present headspace microextraction techniques such as headspace solid-phase microextraction (HS-SPME) and headspace single-drop microextraction (HS-SDME).

Authors+Show Affiliations

College of Environmental and Chemical Engineering, Dalian University, Dalian 116622, PR China.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

19773203

Citation

Meng, Liang, et al. "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." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 877, no. 29, 2009, pp. 3645-51.
Meng L, Liu X, Wang B, et al. 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. J Chromatogr B Analyt Technol Biomed Life Sci. 2009;877(29):3645-51.
Meng, L., Liu, X., Wang, B., Shen, G., Wang, Z., & Guo, M. (2009). 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. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 877(29), 3645-51. https://doi.org/10.1016/j.jchromb.2009.09.006
Meng L, et al. 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. J Chromatogr B Analyt Technol Biomed Life Sci. 2009 Nov 1;877(29):3645-51. PubMed PMID: 19773203.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - 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. AU - Meng,Liang, AU - Liu,Xin, AU - Wang,Bin, AU - Shen,Guijun, AU - Wang,Zhengqiao, AU - Guo,Ming, Y1 - 2009/09/10/ PY - 2009/07/13/received PY - 2009/09/03/revised PY - 2009/09/03/accepted PY - 2009/9/24/entrez PY - 2009/9/24/pubmed PY - 2009/12/23/medline SP - 3645 EP - 51 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 877 IS - 29 N2 - 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. The feasibility of this method was demonstrated by analyzing human urine and saliva samples with spiked recoveries in the range of 92-103.4%. This work provided an efficient alternative to the present headspace microextraction techniques such as headspace solid-phase microextraction (HS-SPME) and headspace single-drop microextraction (HS-SDME). SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/19773203/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_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(09)00636-9 DB - PRIME DP - Unbound Medicine ER -