Determination of Melamine in Fresh Milk with Hollow Fiber Liquid Phase Microextraction Based on Ion-Pair Mechanism Combined with High Performance Liquid Chromatography
(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:
https://lup.lub.lu.se/record/3283244
- author
- Gao, Leihong and Jönsson, Jan Åke LU
- organization
- publishing date
- 2012
- 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
- additional info
- The information about affiliations in this record was updated in December 2015. The record was previously connected to the following departments: Analytical Chemistry (S/LTH) (011001004)
- id
- 329e4f3b-ce75-4f1f-873b-7a610ce44195 (old id 3283244)
- date added to LUP
- 2016-04-01 13:57:51
- date last changed
- 2022-01-27 22:05:59
@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}}, keywords = {{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}}, doi = {{10.1080/00032719.2012.688084}}, volume = {{45}}, year = {{2012}}, }