期刊
ANALYTICA CHIMICA ACTA
卷 650, 期 1, 页码 39-43出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.aca.2009.04.026
关键词
Melamine; Isotope internal standard; Gas chromatography/mass spectrometry (GC/MS); Coupled column; Direct determination; Dairy products
资金
- National Natural Science Foundation of China [20775070]
- Zhejiang Provincial Natural Science Foundation of China [R4080124]
- Zhejiang Qianjiang Project of science and technology [2008R10028]
- Zhejiang Provincial Science and Technology Program [2008F70002]
A coupled capillary column system was developed for the qualitative and quantitative determination of melamine with isotope internal standard in dairy products by gas chromatography/mass spectrometry (GC/MS) without derivatization. A 30 m of DB-5ms ((5%-phenyl)methylpolysiloxane, 0.25 mm i.d., 0.25 mu m df) coupled with a 1.5 m of Innowax (polyethylene glycol, 0.32 mm i.d., 0.25 mu m do by a quartz capillary column connector was introduced as separation column. Three advantages were discussed for the coupled system. The sample was fortified with a ring-labeled C-13(3) N-15(3)-melamine as an isotope internal standard and extracted by 1% of trichloroacetic acid aqueous solution. 2.2% of lead acetate solution was then added to deposit protein in the sample matrix. After purification by cation exchange cartridge, the sample solution was directly injected and detected by GC/MS. A six-point calibration curve ranging from 0.05 to 2 mg kg(-1) of rnelamine in sample was used to establish instrument response. The recovery was 93.9-102% with relative standard deviation from 3.1 to 8.7% when isotope internal standard used. The calculated method detection limit was 0.01 mg kg(-1). (C) 2009 Elsevier B.V. All rights reserved.
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