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作 者:刘兴勇[1] 陈兴连[1] 林涛[1] 王丽[1] 汪禄祥[1] 李茂萱 邵金良[1] Liu Xingyong;Chen Xinglian;Lin Tao;Wang Li;Wang Luxiang;Li Maoxuan;Shao Jinliang(Institute of Agriculture Quality Standards&Testing Technique,Yunnan Academy of Agricultural Science,Kunming 650205)
机构地区:[1]云南省农业科学院质量标准与检测技术研究所,昆明650205
出 处:《中国食品学报》2022年第1期324-331,共8页Journal of Chinese Institute Of Food Science and Technology
基 金:国家自然科学基金地区科学基金项目(31660494)。
摘 要:基于液液-分散固相萃取净化和高效液相色谱仪建立烘焙咖啡中5-羟甲基糠醛定量测定方法。采用1%乙酸-乙腈溶液作为提取溶剂,3.0 g氯化钠+1.0 g乙酸钠为盐析剂,50 mg C_(18)粉+20 mg N-丙基乙二胺+200 mg无水硫镁酸为分散固相萃取净化剂。以Shiseido CAPCELL PAK MG C_(18)色谱柱(150 mm×4.6 mm i.d.,5.0μm)为分析柱,实现5-HMF的分离,以甲醇-水溶液为流动相进行梯度洗脱。在优化条件下,5-HMF在0.5~50.0 mg/L线性范围内线性良好,相关系数为0.9991,检出限为0.01 mg/kg,定量限为0.03 mg/kg,在3个加标水平下,5-HMF的加标回收率为85.50%~105.5%,相对标准偏差为4.28%~7.59%(n=5)。采用本方法测定了烘焙小粒咖啡中5-HMF含量。结果表明:烘焙温度、烘焙时间和烘焙程度,对小粒咖啡中5-羟甲基糠醛含量影响非常明显。A method was developed for the detection of 5-hydroxymethylfurfural in roasting Coffea arabica by high performance liquid chromatography combined with liquid-liquid extraction and dispersive solid phase extraction(DSPE).After extracted with 1.0% acetic acid acetonitrile solution with ultrasound assistance,the samples were pretreated with QuEChERS method including extraction salting-out(3.0 g NaCl + 1.0 g NaAc),purification(50 mg C18+ 20 mg PSA + 200 mg MgSO4).The 5-hydroxymethylfurfural was then purified on a Shiseido CAPCELL PAK MG C18 column(150 mm×4.6 mm,5.0 μm),and gradient elution was conducted using methanol and water solution as the mobile phases.Under the optimum conditions,the calibration curves of the 5-hydroxymethylfurfural showed good linearity(r = 0.9991) within their respective linear ranges.The limits of quantification(LOQs) and limits of detection(LODs) was 0.01 mg/kg(S/N = 10)and 0.03 mg/kg(S/N = 3).The recoveries were in the range of 85.50%-105.5% at three spiked levels,with relative standard deviations of 4.28%-7.59%(n = 5).The results showed that roasting temperature,time and degree play an important role in the 5-HMF content of the final Coffea arabica product.
分 类 号:TS273[轻工技术与工程—农产品加工及贮藏工程]
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