Hydrophilic interaction chromatography/tandem mass spectrometry for the determination of melamine in royal jelly and royal jelly lyophilized powder

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• 作者：Jinhui Zhou ; Jing Zhao ; Xiaofeng Xue ; Jinzhen Zhang ; Fang Chen ; Yi Li ; Liming Wu ; Chenchen Li ; Jianqiu Mi
• 关键词：Melamine ; Hydrophilic interaction chromatography/tandem mass spectrometry ; Royal jelly ; Royal jelly lyophilized powder
• 刊名：Journal of Chromatography B, Analytical Technologies in the Biomedical and Life Sciences
• 出版年：2009
• 出版时间：15 December 2009
• 年：2009
• 卷：877
• 期：32
• 页码：4164-4170
• 全文大小：654 K

文摘

Melamine has become the focus of attention for the possible occurrence of nephrolithiasis and associated deaths, because it was added to foods to increase the apparent protein content by unethical manufacturers. An analytical method based on hydrophilic interaction chromatography/tandem mass spectrometry (HILIC-MS/MS) was developed and validated for the determination of melamine in the royal jelly (RJ) and royal jelly lyophilized powder (RJLP). Trace of melamine was extracted from the RJ and RJLP by ultrasonic-assisted extraction followed by clean-up procedure using mixed-mode cation exchange (MCX) solid phase extraction and separated on a hydrophilic interaction chromatography (HILIC) analytical column with acetonitrile/5 mM ammonium acetate buffer (88:12, v/v) as mobile phase. Detection was carried out by positive electrospray ionization (ESI+) in multiple reaction monitoring (MRM) mode. The chromatographic separation was obtained within 5 min and was linear in the concentration range of 0.01–8 μg/mL in RJ and 0.05–10 μg/mL in RJLP for melamine. The mean extraction recoveries for melamine were ranged from 89.6 to 100.4 % . Method validation parameters were evaluated such as linearity, selectivity, precision, carryover and recovery, giving results within the acceptable range. The proposed method was successfully applied to the quantitation of melamine in RJ and RJLP. This approach will be of particular utility for the evaluation of melamine residue level and routine monitor of melamine in RJ and RJLP samples.