Microsoft Word 王春民 二校 出1813、1817

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1 7 5 Vol. 7 No Journal of Food Safety and Quality May, 王春民 *, 张秋萍, 吴春霞 (, ) 摘要 : 目的 - (ultra performance liquid chromatography- tandem mass spectrometry, UPLC-MS/MS) 方法,, UPLC-MS/MS,, 结果 1~10.0 μg/l, 0.999, 76%, 0. 1 μg/kg, 3.4% (n=6) 结论, 关键词 : - ; ; Determination of residues of metronidazole in honey by ultra performance liquid chromatography-tandem mass spectrometry WANG Chun-Min *, ZHANG Qiu-Ping, WU Chun-Xia (Suzhou Center for Disease Control and Prevention, Suzhou , China) ABSTRACT: Objective To establish a method for the determination of metronidazole in honey samples by ultra performance liquid chromatography-tandem mass spectrometric (UPLC MS/MS). Methods Honey samples were mixed with saturated sodium chloride and extracted with ethyl acetate, and then purified by cation exchange column. The metronidazole residues in the extracts were detected using UPLC MS/MS (ESI+) with multiple reactions monitoring (MRM), and quantitated with external standard method. Results Metronidazole had a good linear relationship in the range of 1~10.0 μg/l with the linear correlation coefficient larger than The recovery was 76%, the limits of detection (LOD) was 0.1 μg/kg, and the relative standard deviation (RSD) was 3.4% (n=6). Conclusion The proposed method is fast, accurate and sensitive, which is suitable for the determination of metronidazole residues in honey samples. KEY WORDS: ultra performance liquid chromatography-tandem mass spectrometric; honey; metronidazole 1 引言 (metronidazole, MTZ),, , 1, (nitroimidazoles) MTZ, [1-5],, [6-8], * 通讯作者 :,, chunminwang@163.com. *Corresponding author: WANG Chun-Min, Senior Engineer, Suzhou Center for Disease Control and Prevention, Suzhou , China. chunminwang@163.com

2 1814 7,, 1998 MTZ [9], 2002 MTZ [10] [11],,, [12],,, [13,14] [15-18] [19] [20-22] -, 1 Fig. 1 The structure of metronidazole 2 材料与方法 2.1 仪器与试剂 UPLC-TQD - ( Waters ); Multi Reax ( Heidolph ); HHS ( ); : RE-85C ( ), V-700 V-855 ( Buchi ); Biofuge Stratos ( Thermo Fisher Scientific ) N-EVAP-24 ( Organomation ) (, ); (HPLC, ACS ); (, Merck ); ( >99%, ); ; OASIS MCX (60 mg, 3 ml, Waters ) 2.2 材料, 60, 2.3 实验方法 样品前处理 10 g ( 0.01 g) 50 ml, 10 ml,, 15 ml, 20 min, 5 min, 5000 r/min 5 min, 100 ml 15 ml,, 50 4 ml, MCX 3 ml 3 ml 0.1 mol/l 3 ml, ;, 3 ml 0.1 mol/l 2 ml 2% : (95: 5, V:V) 3 ml, 2 min, 3 ml : : (80:20:2, V:V:V), 45, 5 mmol/l : (9: 1, V:V) 1 ml, r/min 5 min 标准溶液配制 (0.10 mg/ml): 10.0 mg, 100 ml,, 0.10 mg/ml,,, μg/l 仪器条件 : ACQUITY UPLC BEH C 18 (2.1 mm 100 mm, 1.7 µm);, 0.3 ml/min, μl 表 1 梯度洗脱程序 Table 1 Gradient elution program /min /% /% (2) : ESI+, (capillary)3.5 kv; (extractor)3.0 V; (source temp)150 ; (desovation temp)350 ; (desolvation gas flow)800 L/h; (LM resolution): LM 1= LM 2=10.0, (HM resolution): HM 1=14.4, HM 2=14.8; (multiple reaction monitoring, MRM) 3 结果与分析 3.1 前处理条件优化 样品制备过程优化,,

3 5, : ,,, ;,,, 60, 样品净化过程优化,,,,, 3 ml,,, 50, 1 ml 5 mmol/l : (9: 1, V:V), 1 min, r/min 5 min,,, 3.2 基质效应分析,,,, : (1),, (2),, (3),,, (4),,,,,, (5),, 3.3 扫描离子的选择,,, 2 表 2 MRM 检测参数 Table 2 Parameters of MRM (s) (V) (V) 1: > : > 128.0* 线性范围 方法检出限和空白试验 μg/l,, Y= X , 0.999,, 2.3.1, 2.3.3, μg/kg,,, 2 MRM Fig. 2 MRM mass spectrums of metronidazole detected in honey samples 172> min 172> min

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