HPLC Determination of Trace Amount of Formaldehyde in Wine Pre-derivatized by Hantzsch Reaction
摘 要
提出了Hantzsch反应衍生-高效液相色谱法测定酒中的微量甲醛的方法。优化的衍生反应条件如下:① 反应体系pH为5.5;② 反应温度为50 ℃;③ 反应时间为20 min;④ 衍生剂乙酰丙酮(0.2+100)溶液用量为0.5 mL;⑤ 氯化铵溶液浓度0.5 mol·L-1。甲醛质量浓度在2~2 000 μg·L-1范围内与峰面积呈线性关系,方法的检出限(3S/N)为0.2 μg·L-1。方法用于啤酒和白酒样品的分析,加标回收率在81.2%~102%之间。
Abstract
A method of HPLC for determination of trace amount of formaldehyde in wine with derivatization by Hantzsch reaction was proposed. The optimized conditions for derivatization reaction found were as follows: ① acidity of the reaction system: pH 5.5; ② temperature of reaction: 50 ℃; ③ time of reaction: 20 min; ④ amount of acetylacetone (0.2+100) solution added: 0.5 mL; ⑤ concentration of ammonium chloride solution acidity: 0.5 mol·L-1. Linear relationship between values of peak area and mass concentration of formaldehyde was kept in the range of 2-2 000 μg·L-1, with detection limit (3S/N) of 0.2 μg· L-1.The proposed method was applied to the analysis of samples of beer and white spirit, giving values of recovery by standard addition method in the range of 81.2%-102%.
中图分类号 O652.63
所属栏目 工作简报
基金项目 河南省杰出青年计划(124100510003);河南省基础与前沿项目(122300410241);环境化学与生态毒理学国家重点实验室开放基金(KF2010-13)
收稿日期 2013/6/8
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备注徐莉莉(1984-),女,河南周口人,硕士研究生,主要研究方向为环境化学。
引用该论文: XU Li-li,TAI Chao,WU Li,ZHAO Tong-qian,HAN Dan. HPLC Determination of Trace Amount of Formaldehyde in Wine Pre-derivatized by Hantzsch Reaction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(1): 27~30
徐莉莉,邰超,武俐,赵同谦,韩丹. Hantzsch反应衍生-高效液相色谱法测定酒中微量甲醛[J]. 理化检验-化学分册, 2014, 50(1): 27~30
被引情况:
【1】赵龙,钟瑞华,李腾峰,卢成,杨慧明, "高效液相色谱法测定汽车内饰件中的甲醛、乙醛和丙酮",理化检验-化学分册 52, 1194-1196(2016)
【2】赵龙,钟瑞华,李腾峰,卢成,杨慧明, "高效液相色谱法测定汽车内饰件中的甲醛、乙醛和丙酮",理化检验-化学分册 52, 1194-1196(2016)
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参考文献
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【8】LI Jian-rong, ZHU Jun-li, YE Li-fang. Determination of formaldehyde in squid by high-performance liquid chromatography[J]. Asia Pacific Journal of Clinical Nutrition, 2007,16:127-130.
【9】LO K M, YUNG Y L. Integration of headspace solid phase micro-extraction with gas chromatography for quantitative analysis of formaldehyde[J]. Bulletin of the Korean Chemical Society, 2013,34(1):139-142.
【10】顾秀英,鲍忠定,许荣年,等.衍生气相色谱法测定啤酒中的甲醛[J].食品研究与开发, 2008,29(6):116-118.
【11】彭锦峰,刘景富,吕爱华,等.HPLC法测定食用香菇中的甲醛[J].分析试验室, 2005,24(4):57-59.
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【2】GB/T 5009.49-2003中华人民共和国国家标准[S].
【3】NY/T 273-2012中华人民共和国农业行业标准[S].
【4】王圣庆,郭瑛,马言顺,等.柱前衍生高效液相色谱法测定啤酒中微量甲醛[J].化学研究与应用, 2006,18(2):214-216.
【5】叶青,魏培莲,尤玉如,等.HPLC法直接测定啤酒中微量甲醛方法的研究[J].食品与发酵工业, 2006,32(9):126-129.
【6】陈笑梅,施旭霞,朱卫建,等.高效液相色谱直接测定甲醛衍生物反应条件的研究[J].分析化学, 2004,32(11):1489-1491.
【7】SOMAN A, QIU Y, LI Q C. HPLC-UV method development and validation for the determination of low level formaldehyde in a drug substance[J]. Journal of Chromatographic Science, 2008,46(6):461-465.
【8】LI Jian-rong, ZHU Jun-li, YE Li-fang. Determination of formaldehyde in squid by high-performance liquid chromatography[J]. Asia Pacific Journal of Clinical Nutrition, 2007,16:127-130.
【9】LO K M, YUNG Y L. Integration of headspace solid phase micro-extraction with gas chromatography for quantitative analysis of formaldehyde[J]. Bulletin of the Korean Chemical Society, 2013,34(1):139-142.
【10】顾秀英,鲍忠定,许荣年,等.衍生气相色谱法测定啤酒中的甲醛[J].食品研究与开发, 2008,29(6):116-118.
【11】彭锦峰,刘景富,吕爱华,等.HPLC法测定食用香菇中的甲醛[J].分析试验室, 2005,24(4):57-59.
【12】JONES S B, TERRY C M, LISTER T E, et al. Determination of submicromolar concentrations of formaldehyde by liquid chromatography[J]. Analytical Chemistry, 1999,71(18):4030-4033.
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