Tsai Chia-Fen, Wu Guan-Yan, Kuo Ching-Hao, Lin Yung-Wei, Chang Chun-Hsiung, Tseng Su-Hsiang, Kao Ya-Min, Chiueh Lih-Ching, Lu Ting-Jang, Shih Daniel Yang-Chih
Department of Food Chemistry, Food and Drug Administration, Ministry of Health and Welfare, Taipei, Taiwan.
Institute of Food Science and Technology, National Taiwan University, Taipei, Taiwan.
J Food Drug Anal. 2015 Sep;23(3):442-446. doi: 10.1016/j.jfda.2014.09.002. Epub 2015 Jan 2.
A high-performance liquid chromatography (HPLC) method was developed for the determination of maleic acid which was released from starch maleate (SM) through the alkaline hydrolysis reaction. The proper alkaline hydrolysis conditions and LC separation are reported in this study. The starch samples were treated with 50% methanol for 30 minutes, and then hydrolyzed by 0.5N KOH for 2 hours to release maleic acid. A C18 column and gradient mobile phase consisting of 0.1% phosphoric acid and methanol at a flow rate of 1.0 mL/minute were used for separation. The method showed a good linearity in the range of 0.01-1.0 ìg/mL, with a limit of quantification (LOQ) at 10 mg/kg in starch. The recoveries in corn starch, noodle, and fish balls were between 93.9% and 108.4%. The relative standard deviation (RSD) of precision was <4.9% (n = 3). This valid method was rapid, sensitive, precise, and suitable for routine monitoring of the illegal adulteration of SM in foods.
建立了一种高效液相色谱(HPLC)法,用于测定马来酸淀粉酯(SM)在碱性水解反应中释放出的马来酸。本研究报道了合适的碱性水解条件和液相色谱分离方法。淀粉样品用50%甲醇处理30分钟,然后用0.5N氢氧化钾水解2小时以释放马来酸。采用C18柱和由0.1%磷酸和甲醇组成的梯度流动相,流速为1.0 mL/分钟进行分离。该方法在0.01-1.0 μg/mL范围内具有良好的线性,淀粉中的定量限(LOQ)为10 mg/kg。玉米淀粉、面条和鱼丸中的回收率在93.9%至108.4%之间。精密度的相对标准偏差(RSD)<4.9%(n = 3)。该有效方法快速、灵敏、精确,适用于食品中SM非法掺假的常规监测。