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1 5 1 Vol. 5 No Journal of Food Safety and Quality Jan., 2014 惠芸华, 于 * 欢, 于慧娟 (, ) 摘要 : 目的方法, FMOC-CL 结果 45 1 h 50 μg FMOC-CL V :V KH2 PO 4 =2:1 结论, 关键词 : ; ; Study on optimization of derivatization reaction conditions during determination of erythromycin residues HUI Yun-Hua, YU Huan, YU Hui-Juan * (Ministry of Agriculture Supervision and Testing Center for Aquatic Products, East China Sea Fisheries Research Institute, Chinese Academy of Fishery Science, Shanghai , China) ABSTRACT: Objective To investigate the conditions of derivatization reaction during the process of erythromycin determination in aquatic products. Methods The reaction temperature, reaction time, FMOC-CL quantity and reaction system were studied to optimize the derivatization reaction. Results The results showed that the best derivatization reaction conditions of erythromycin were as follows: the derivatization reaction temperature was 45, the reaction time was 1 h, and the amount of FMOC-CL was 50 μg under the reaction system of V acetonitrile :V KH2PO4 =2:1. Conclusion suitable for the established experiment. KEY WORDS: erythromycin; derivatization reaction; optimization The derivatization reaction condition was (erythromycin), [1-2],, (Aristichys nobilis) (Hypophthalmichthys molitrix) [3],, [4-9],, [10],,,,, 9- * 通讯作者 :,, [email protected] *Corresponding author: YU Hui-Juan, Researcher, East China Sea Fisheries Research Institute, Chinese Academy of Fishery Science, No.300, Jungong Road, Shanghai , China. [email protected]

determination of erythromycin residues HUI Yun-Hua, YU Huan, YU Hui-Juan * (Ministry of Agriculture Supervision and Testing Center for Aquatic Products, East China Sea Fisheries Research Institute,

2 90 5 (FMOC-CL), [11] FMOC-CL, FMOC-CL, 1 1 Fig. 1 The derivation reaction of erythromycin 1 材料与方法 1.1 仪器和试剂 (organomation), (MSI IKA), Agilent1100, (101-2B, ), TSQ Quantum ; (Fisher, ), ( ), ( ), ( ), ( ), : 99%(SIGMA ), : 99%(SIGMA ), 9- (FMOL-CL): 98%(SIGMA ) 1.2 溶液配制 : g, 100 ml, 100 μg/ml,, 10 μg/ml FMOL-CL : FMOL-CL, 100 ml 1.3 实验方法 1, 3 3, 3, 15 min, 不同反应温度对红霉素衍生化程度的影响不同反应时间对红霉素衍生化程度的影响 min 不同量的衍生试剂对红霉素衍生化程度的影响 μg FMOC-CL, 不同反应体系对红霉素衍生化程度的影响 V :V KH2 PO 4 =1:1, V :V KH2 PO 4 =2:1, V :V KH2 PO 4 =3:1, V :V KH2 PO 4 =4:1, V :V KH2 PO 4 =5: 高压液相色谱分析条件 : : CAPCELL PAK MGⅡ-C 18 (4.6 mm 150 mm) : A: ; B: 0.03 mol/l (ph 6.3) 1 : 40 : 2 ml/min : 50 μl : 255 nm; : 315 nm Table 1 (min) 表 1 梯度洗脱程序 The gradient elution procedure A(%) B(%)

0100 g, 100 ml, 100 μg/ml,, 10 μg/ml FMOL-CL : FMOL-CL, 100 ml 1.3 实验方法 1, 3 3, 3, 15 min, 1.3.1 不同反应温度对红霉素衍生化程度的影响 30 35 40 45 50 55 60 1.3.2 不同反应时间对红霉素衍生化程度的影响 30 60 90 120 min 1.

3 1, : 91 2 结果与讨论 2.1 反应温度对红霉素衍生化程度的影响 2,,, 40~50, 反应时间对红霉素衍生化程度的影响 3, 60~90 min,, 2.3 不同量的反应试剂对红霉素衍生化程度的影响 4,,, 50 μg,, 4 FMOC-CL (n=3) Fig. 4 The effect of amount of FMOC-CL on erythromycin 2.4 不同反应体系对红霉素衍生化程度的影响 5, V :V KH2 PO 4 =2:1,, 2 (n=3) Fig. 2 The effect of reaction temperature on erythromycin 5 (n=3) Fig. 5 The effect of ratio of acetonitrile to KH 2 PO 4 on : : 40~50, 3 (n=3) Fig. 3 The effect of reaction time on erythromycin : 1 h, : 50 μg, V :V KH2 PO 4 =2:1,, min, min

4 不同反应体系对红霉素衍生化程度的影响 5, V :V KH2 PO 4 =2:1,, 2 (n=3) Fig. 2 The effect of reaction temperature on erythromycin 5 (n=3) Fig.

4 92 5 Fig. 6 6 HPLC chromatogram of erythromycin and roxithromycin standard 参考文献 [1]. [J]., 2000, 35(3): Ren CZ. The progress of structure-activity relationship study on erythromycin and its derivatives[j]. Chin J Vet Med, 2000, 35(3): [2]. [J]., 2005, 14(19): Yuan TS. Progress in research and application of macrolide antibiotics [J]. Mod J Integr Tradit Chin Western Med, 2005, 14(19): [3]. [J]., 2004, (6): 31. Cao FX. Application of antibiotics in fish production[j]. World of Breeding, 2004: 31. [4],,. [J]., 2004, 23(8): Zhao HM, Jiang XM, Lin XF. Current status on residues of antibiotics in seafood [J]. Fisheries Sci, 2004, 23(8): [5] Billedeau SM, Heinze TM, Siitonen PH. Liquid chromatography analysis of erythromycin in salmon tissue by electrochemical detection with confirmation by electrospray ionization mass spectrometry [J]. J Agric Food Chem, 2003, 51(6): [6] Dreassi E, Corti P, Bezzini F. High-performance liquid chromatography assay of erythromycin from biological matrix using electrochemical or ultraviolet detection [J]. Analyst, 2000, 125: [7],. [J]., 2003, 24(2): Han NY, Zhou T. Determination of erythromycin residues in honey[j]. Food Sci, 2003, 24(2): [8] Xiao WT, Chen B, Yao SZ, et al. Simultaneous determination of erythromycin propionate and base in human plasma by high performance liquid chromatography-electrospray mass spectrometry [J]. J Chromatogr B, 2005, (817): [9],,. - [J]., 2013, (6): Zhou L, Wu LM, Zhou JH. Determination of Erythromycin Residues in Honeycomb by High Performance Liquid Chromatography-Tandem Mass Spectrometry [J]. J Chin Inst Food Sci Technol, 2013, (6): [10],,,. [J]., 2009, 28(11): Hui YH, Cai YQ, Sheng XS, et al. A high performance uquid chromatographic method for the determination of erythromycin residues in aquatic products[j]. Chin J Anal Lab, 2009, 28(11): [11] Edder P, Coppex L, Cominoli C. Analysis of erythromycin and oleandomycin residues in food by high-performance liquid chromatography with fluorometric detection [J]. Food Addit Contam, 2002, 19(3): ( 责任编辑 : 赵静 )

Progress in research and application of macrolide antibiotics [J]. Mod J Integr Tradit Chin Western Med, 2005, 14(19): 2620 2621. [3]. [J]., 2004, (6): 31. Cao FX.

5 1, : 93 作者简介惠芸华, 助理研究员, 主要研究方向为水产品质量安全管理水产品中渔药残留及生物毒素检测技术和渔药在生物体中富集及代谢规律 [email protected] 于慧娟, 教授, 主要研究方向为水产品质量安全管理水产品中渔药残留及生物毒素检测技术和渔药在生物体中富集及代谢规律 [email protected] 转基因食品安全专题征稿 30, 2001 SCI 14 ISO 投稿方式 : [email protected] 食品安全质量检测学报编辑部