Microsoft Word 官咏仪-二校 2247

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1 8 6 Vol. 8 No Journal of Food Safety and Quality Jun., 2017 官咏仪 1, 邱志超 2*, 金梦 1, 宋阳 1, 张美金 1, 陈毓芳 1, 谢玉珊 (1., ; 2., ) 1 摘要 : 目的 方法, Agilent TC-C 18, -, 结果 4 4, 88.1%~97.7%, 2.47%~5.72%, 0.10 mg/kg; 84.5%~104%, 1.21%~5.28%, 0.05 mg/kg 结论, 关键词 : ; ; Simultaneous determination of natamycin and dimethyl fumarate in foods by high performance liquid chromatography GUAN Yong-Yi 1, QIU Zhi-Chao 2*, JIN Meng 1, SONG Yang 1, ZHANG Mei-Jin 1, CHEN Yu-Fang 1, XIE Yu-Shan 1 (1. Inspection and Quarantine Technology Center, Guangdong Entry-Exit Inspection and Quarantine Bureau, Guangzhou , China; 2. Guangzhou Quality Supervision and Testing Institute, Guangzhou , China) ABSTRACT: Objective To establish a method for simultaneous determination of natamycin and dimethyl fumarate (DMF) in foods by high performance liquid chromatography (HPLC). Methods Samples were extracted by methanol and water, separated by Agilent TC-C 18 column, detected by HPLC with photo-diode array detector (PDA) and quantified by the external standard method. Results At 4 different spiked levels in 4 kinds of food, the average recoveries of natamycin were between 88.1%~97.7%, with the RSD of 2.47%~5.72%. The average recoveries of dimethyl fumarate were between 84.5%~104%, with the RSD of 1.21%~5.28%. Detection limits of natamycin and DMF were 0.10 mg/kg and 0.05 mg/kg, respectively. Conclusion This method is simple, fast and accurate, which can be applied to the analysis of the content of natamycin and DMF in foods. KEY WORDS: high performance liquid chromatography; natamycin; dimethyl fumarate 1 引言 (natamycin),,,,,,, * 通讯作者 :,,, @qq.com *Corresponding author: QIU Zhi-Chao, Master, Quality Engineer, Guangzhou Quality Supervision and Testing Institute, No.1-2, Zhujiang Road, Chao Tian Industrial Zone, Shilou Town, Panyu District, Guangzhou , China @qq.com

2 6, : 2247, [1,2] GB , 10 mg/kg [3] (dimethyl fumarate, DMF),,,, [4,5],,,, [5] , ( )(20095 ) [6],, [7] - [8] [9] [10] [11] - [5] [12] - [13] [14] [15-17],,,,, 2 材料与方法 2.1 仪器与试剂 Waters alliance e2695 (, Waters ); BT 124S ( Sartorius ); SW 30H ( SONO SWISS ); Multi Reax ( Heidolph ); 4K15 ( Sigma ); ( 0.22 μm) (, Thermo Fisher Scientific ); ( Mill-Q ); ( 91.1%, ); ( 99.5%, Dr.Ehrenstorfer ) 2.2 实验方法 标准溶液的配制 25 mg, :(1:1, V:V) 25 ml, 1000 mg/l, -20, :(1:1, V:V) 100 mg/l, :(1:1, V:V) mg/l 样品前处理 5.00 g 50 ml, 30 ml, 10 min 15 min 50 ml, 30 min, r/min 5 min, 0.22 μm, 色谱条件 : Agilent TC-C 18 (250 mm 4.6 mm, 5 μm); :(65:35, V:V); 0.8 ml/min; 25 ; 20 μl; 218 nm 2.3 数据处理和统计方法 Empower3, 4 4, 2 6,, 3 结果与分析 3.1 分析条件的优化 流动相的选择, - ---, ph, :(65:35, V:V) 1,, 2 4,, 50 mg/l,,, ;,, 3, 80%, 检测波长的选择 20 μl 20 mg/l, 200~310 nm ( 3), 210 nm 303 nm, 215~225 nm,, 10 5,

3 2248 8,, 218 nm 提取溶液的选择 [15], :(1:20, V:V) ph [11], [16], ph,, :(65:35, V:V),, 0.05 mg/kg 0.10 mg/kg 加标回收率及相对标准偏差, 4 6 1, 88.1%~97.7%, 2.47%~5.72%; 84.5%~104%, 1.21%~5.28% 3.2 方法学验证 标准曲线及检出限 0.1~20.0 mg/l,, Y= X , Y= X , r 0.999,, 3, 1: (dimethyl fumarate); 2: (natamycin) 1 (20 mg/l) Fig.1 Chromatogram of dimethyl fumarate and natamycin standard (20 mg/l) Fig. 2 1: (dimethyl fumarate); 2: (natamycin) 2 (50 mg/l) Chromatograms of dimethyl fumarate and natamycin spiked samples (50 mg/l)

4 6, : 2249 Fig. 3 3 Response signal values of different detected wavelengths 表 1 4 种基质中纳他霉素和富马酸二甲酯的加标回收率和相对标准偏差 (n=6) Table 1 Results of recoveries and relative standard deviations of natamycin and dimethyl fumarate in 4 kinds of food (n=6) (mg/kg) 4 结论 (%) (%) (%) (%) ,,,,, 参考文献 [1],,,. (natamycin) [J]., 2007, 3(45): Yue HB, Yue XQ, Li J, et al. The characteristics, application, production and research status of natamycin [J]. Food Sci Technol, 2007, 3(45): [2],,,. [J]., 2010, 4(79): , 373. Yan YZ, Zhou XX, Li WF, et al. Antimicrobial mechanism and the application of natamycin in food [J]. Sci Technol Food Ind, 2010, 4(79): , 373. [3] GB [S]. GB National food safety standard for uses of food additives [S]. [4],,. [J]., 2008, (7): Han YH, Tang Z, Han P. Synthesis of new food preservative named dimethyl fumarate [J]. Chem Eng Equip, 2008, (7): [5],,,. - [J]., 2014, 42(21): , Tang LN, Ning HY, Zeng XY, et al. Determination of dimethyl fumarate in cake by ultra high performance liquid chromatography-tandem mass [J]. J Anhui Agric Sci, 2014, 42(21): , [6] ()[Z]. List of illegal additives maybe add in foods (second batch) [Z]. [7],,,. [J]., 2012, (08): 8687, 91. Zhang H, Wu Y, Zhu L, et al. Determination of natamycin in various

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