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Determination of Melamine in Fresh Milk with Hollow Fiber Liquid Phase Microextraction Based on Ion-Pair Mechanism Combined with High Performance Liquid Chromatography

Gao, Leihong and Jönsson, Jan Åke LU (2012) In Analytical Letters 45(16). p.2310-2323
Abstract
In this work, a novel analytical method based on hollow fiber liquid phase microextraction (HF-LPME) and high performance liquid chromatography (HPLC) was developed for the analysis of melamine in fresh milk. The conditions of the HF-LPME were investigated and optimized. As a result, a supported liquid membrane containing 6-undecanone and di-2-ethylhexyl phosphoric acid (D2EHPA) was selected. The extractions were made from 25 mL aqueous donor phase (prepared from milk) with pH 5.0 to a more acidic acceptor phase (36 mu L 1 M HCl) and the mass transfer was driven by the proton gradient between these phases. Other optimum conditions of the HF-LPME were 60 min extraction time at 360 rpm stirring rate and an extraction factor of 21 times... (More)
In this work, a novel analytical method based on hollow fiber liquid phase microextraction (HF-LPME) and high performance liquid chromatography (HPLC) was developed for the analysis of melamine in fresh milk. The conditions of the HF-LPME were investigated and optimized. As a result, a supported liquid membrane containing 6-undecanone and di-2-ethylhexyl phosphoric acid (D2EHPA) was selected. The extractions were made from 25 mL aqueous donor phase (prepared from milk) with pH 5.0 to a more acidic acceptor phase (36 mu L 1 M HCl) and the mass transfer was driven by the proton gradient between these phases. Other optimum conditions of the HF-LPME were 60 min extraction time at 360 rpm stirring rate and an extraction factor of 21 times (extraction efficiency 3%) was obtained. The C8 column was operated at 1 mL/min at room temperature and the UV detection wavelength was 240 nm for HPLC. The mobile phase was 10 mM sodium n-octanesulfonate (pH 3.0) mixed with acetonitrile (85:15, v/v). The relative recovery of melamine for milk samples spiked with 0.5-25 mg/kg was in the range of 89.1-120.6% with the RSDs (n = 4) of 4.0-8.5%. It was found that the proposed method provided a linear range from 0.1 to 50 mg/kg (r(2) = 0.9993), method detection limit (MDL) of 0.003 mg/kg and method quantification limit (MQL) of 0.01 mg/kg. The obtained results demonstrated that HF-LPME combined with HPLC is a simple and cheap method for the determination of melamine in fresh milk. (Less)
Please use this url to cite or link to this publication:
author
organization
publishing date
type
Contribution to journal
publication status
published
subject
keywords
HF-LPME, Hollow fiber liquid phase microextraction, HPLC, Melamine, Milk
in
Analytical Letters
volume
45
issue
16
pages
2310 - 2323
publisher
Taylor & Francis
external identifiers
  • wos:000310613800004
  • scopus:84868159373
ISSN
0003-2719
DOI
10.1080/00032719.2012.688084
language
English
LU publication?
yes
id
329e4f3b-ce75-4f1f-873b-7a610ce44195 (old id 3283244)
date added to LUP
2012-12-20 12:28:06
date last changed
2017-05-28 04:03:11
@article{329e4f3b-ce75-4f1f-873b-7a610ce44195,
  abstract     = {In this work, a novel analytical method based on hollow fiber liquid phase microextraction (HF-LPME) and high performance liquid chromatography (HPLC) was developed for the analysis of melamine in fresh milk. The conditions of the HF-LPME were investigated and optimized. As a result, a supported liquid membrane containing 6-undecanone and di-2-ethylhexyl phosphoric acid (D2EHPA) was selected. The extractions were made from 25 mL aqueous donor phase (prepared from milk) with pH 5.0 to a more acidic acceptor phase (36 mu L 1 M HCl) and the mass transfer was driven by the proton gradient between these phases. Other optimum conditions of the HF-LPME were 60 min extraction time at 360 rpm stirring rate and an extraction factor of 21 times (extraction efficiency 3%) was obtained. The C8 column was operated at 1 mL/min at room temperature and the UV detection wavelength was 240 nm for HPLC. The mobile phase was 10 mM sodium n-octanesulfonate (pH 3.0) mixed with acetonitrile (85:15, v/v). The relative recovery of melamine for milk samples spiked with 0.5-25 mg/kg was in the range of 89.1-120.6% with the RSDs (n = 4) of 4.0-8.5%. It was found that the proposed method provided a linear range from 0.1 to 50 mg/kg (r(2) = 0.9993), method detection limit (MDL) of 0.003 mg/kg and method quantification limit (MQL) of 0.01 mg/kg. The obtained results demonstrated that HF-LPME combined with HPLC is a simple and cheap method for the determination of melamine in fresh milk.},
  author       = {Gao, Leihong and Jönsson, Jan Åke},
  issn         = {0003-2719},
  keyword      = {HF-LPME,Hollow fiber liquid phase microextraction,HPLC,Melamine,Milk},
  language     = {eng},
  number       = {16},
  pages        = {2310--2323},
  publisher    = {Taylor & Francis},
  series       = {Analytical Letters},
  title        = {Determination of Melamine in Fresh Milk with Hollow Fiber Liquid Phase Microextraction Based on Ion-Pair Mechanism Combined with High Performance Liquid Chromatography},
  url          = {http://dx.doi.org/10.1080/00032719.2012.688084},
  volume       = {45},
  year         = {2012},
}