高效液相色谱法快速测定葡萄制品中3种糠醛类物质.docVIP

高效液相色谱法快速测定葡萄干中3种糠醛类物质 汪辉1，黎瑛2，夏立新1，彭新凯1，李秀娟3，袁靖2 （1. 长沙市食品质量安全监督检测中心，长沙 410013；2. 湖南省食品安全生产工程技术研究中心，长沙 410013；3. 新疆吐鲁番地区质量与计量检测所，吐鲁番 838000） 摘要：建立高效液相色谱法快速测定葡萄干中3种糠醛类物质。甲醇-0.02 mol/L醋酸铵（用冰醋酸调pH=3.5）（20+80）溶液分析时流动相A为0.02 mol/L醋酸铵（用冰醋酸调pH=3.5），B为甲醇，对目标化合物进行梯度洗脱。流速为1.0 mL/minC18色谱柱分离，柱温为40℃，检测波长为285 nm。5-羟甲基糠醛、糠醛、5-甲基糠醛在0.7-500 mg/L浓度范围内线性良好，方法检出限分别为0.4, 0.5, 0.3 mg/kg, 回收率在9-109%之间，相对标准偏差在4.%以下。该方法前处理过程简单，快速、准确，适于同时快速测定葡萄干中3种糠醛类物质。 关键词：高效液相色谱法葡萄干5-羟甲基糠醛糠醛5-甲基糠醛 中图分类号： 文献标志码： 文章编号： Rapid etermination of Three Furfurals in Raisin by High Performance Liquid Chromatography WANG Hui1, LI Ying2, XIA Li-xin1, PENG Xin-kai1, LI Xiu-juan3, YUAN Jing2 (1. Changsha Center of Supervision and Inspection on Food Quality Safety, Changsha 410013 China; 2. Food safety production Engineering Research Center of Hunan Province Changsha 410013, China; 3. Xinjiang Turpan area testing institute of quality and metrology, Tulufan 838000, China) Abstract: A method of high performance liquid chromatography was developed for rapid determination of three furfurals in raisin. The samples were extracted by the solution of 0.02 mol/L ammonium acetate(pH=3.5) using ultrasonic, then, centrifuged. After filtered through 0.45 μm filters, the filtrate would be analyzed by high performance liquid chromatography. Mobile phase A was 0.02 mol/L ammonium acetate(pH=3.5) and the mobile phase B was methanol with current velocity of 1.0 mL/min. Under gradient elution, the target compounds were separated by C18 column at 40℃ which were detected on 285 nm. The calibration curves showed good linearity for 5-hydroxymethylfurfural, furfural and 5-methylfurfural in the range of 0.7-500 mg/L. The limits of detection of three target compounds were 0.4, 0.5, 0.3 mg/kg, respectively. The spiked recoveries ranged from 90.3% to 109% with RSDs less than 4.59%. This proposed method was simple pretreatment, rapid and accurate which was suitable for determination of three furfurals in raisin. Key word: H