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1 6 8 Vol. 6 No Journal of Food Safety and Quality Aug., 2015 付艳梅 *, 王海霞, 张秀丰 (, ) 摘要 : 目的方法 1% -, MCX,, C 18, -, 274 nm, 结果 mg/l,, , 0.02 mg/kg, 85.2% 95.9% 结论, 关键词 : ; ; ; Determination of carbendazim residue in fried broad bean by high performance liquid chromatography FU Yan-Mei *, WANG Hai-Xia, ZHANG Xiu-Feng (Hengshui Entry-Exit Inspection and Quarantine Bureau, Hengshui , China) ABSTRACT: Objective To study and establish a method for determination of carbendazim residue in fried broad bean by high performance liquid chromatography. Methods The sample was extracted by 1% acetic acid-acetonitrile, cleaned up by MCX SPE, dissolved and volumed by methanol, and then separated by C 18 chromatography column, the mobile phase was acetonitrile-water, the detection wavelength was 274 nm, and the quantitave method was the external standard method. Results The linear relationship between peak area and concentration was good over the range of 0.10~4.0 mg/l with the correlation coefficient , and the detection limit was mg/kg, the average recoveries of the method were ranged from 85.2%~95.9%. Conclusion This method is easier, faster and suitable for the determination of carbendazim in fried broad bean. KEY WORDS: high performance liquid chromatography; fried broad bean; carbendazim; solid-phase extraction 1 引言,, [1],, [2],,, [3,4], * 通讯作者 :,, fuyanmei013@126.com *Corresponding author: FU Yan-Mei, Assistant Engineer, Hengshui Entry-Exit Inspection and Quarantine Bureau, No. 1396, Renmin Road, Hengshui , China. fuyanmei013@126.com

2 8, : 3279 [5,6], [7-10] - [11] [12] - [13], -,,,,, 2 仪器与方法 2.1 主要仪器与试剂 (e2695, ), ; (6 cc, 150 mg, Waters Oasis) (100 µg/ml), ; (, J.T.Baker ),, 2.2 色谱条件 Welch Ultimate XB-C 18 (250 mm 4.6 mm, 5 µm); : - (85:15, V:V); 274 nm; 1.0 ml/min; 40 ; : 10 µl 2.3 标准溶液的配制 100 µg/ml 10 µg/ml, 10 µg/ml µg/ml 2.4 样品前处理样品的制备,, 样品提取 10 g ( 0.01 g) 50 ml, 40 ml 1% - 1 min, 4000 r/min 5 min, 样品净化 10 ml, 3 ml 1% - MCX, 3 ml, 3 ml, 3 ml 5% -, 45 1 ml, 0.45 µm, 3 结果与分析 3.1 样品前处理条件的优化溶剂的选择,,,,, 1% - 1% -, 1% -,, 60%, 1% -, 85%, 1% - [14] 净化方法的选择, Oasis MCX [15] 3 ml 1% -,, 色谱条件的优化 ( 流动相的选择 ) (ph=6.8) 80:20 85:15,,,,,, 3.2 工作曲线与检出限 ~4.0 mg/l,, Y=28266X-30, r 2 = (S/N=3), 0.02 mg/kg 回收率与精密度 10 g, mg/kg 3, 1, 2, 3

3 Fig. 1 1 HPLC chromatogram of carbendazim standards Fig. 2 2 HPLC chromatogram of the blank sample Fig. 3 3 HPLC chromatogram of blank samples spike

4 8, : 3281 Table 1 表 1 回收率实验 Recoveries of the measured results mg/kg mg/kg % /% RSD% % % % 结论,,, 1% -,,, 参考文献 [1], ( 2 )[M]. :, Liu QK, Zhu KN New pesticide manual (Version 2) [M]. Shanghai: Shanghai Scientific and Technical Publishers, [2]. [J]., 1992, 19(1): Wu LM. Effects of carbendazim on sperm morphology and reproductive ability of male mice [J]. China Occup Med, 1992, 19(1): [3]. [J]., 2015, (05): 30. Ji HC. The occurrence and control measures of favism [J]. Mod Rural Sci Technol, 2015, (05): 30. [4]. [J]., 2015, (05): Zhang XL. Occurrence and control measures of insect pests in green bean [J] Pestic Market News, 2015, (05): 30. [5] GB/T [S] GB/T Determination of carbendazim residues in fruits and vegetables-hplc method [S]. [6] NY/T [S]. NY/T Determination of carbendazim and other 3 benzimidazoles in vegetable and fruit by HPLC [S]. [7],,. - [J]., 2007, 26(5): Kong XH, Hai Y, Qiu NX Solid phase extraction and high performance liquid chromatography method for determination of carbendazim residue in concentrated juice [J] Assay Lab, 2007, 26(5): [8], ( ),,. [J]., 2004, 24(4): Gao R, Zhao R (Wang Z), Yang J, et al. Determination of residues of carbendazim in rapeseed by HPLC [J]. J Nanjing Med Univ, 2004, 24(4): [9],,,. [J]., 2013, (35): Feng JM, Zhang XZ, Feng L, et al. Determination of residues of carbendazim in spinach by HPLC [J]. Agric Mach, 2013, (35): [10],,,. / - [J]., 2014, 5(11): Zhou XJ, Zhao LZ, Xia X, et al. Determination of trace carbendazim in citrus by high performance liquid chromatography with on-line clean-up and solid phase extraction [J] J Food Saf Qual, 2014, 5(11): [11] GB/T [S]. GB/T Determination of thiophanate-methyl, carbendazim in vegetables and fruits [S]. [12],,. [J]., 2008, 25(3): Li BN, Wang YL, Jia JP. Determination of the solid phase micro extraction gas chromatography for the determination of carbendazim in fruits [J]. J Environ Health, 2008, 25(3): [13],,,. LC-MS/MS 2- [J]., 2012, 33(22): 56 59, 62.

5 Huang WW, Liu XS, Zheng L, et al. Determination of residues of 2-Aminobenzimidazole, carbendazim, thiabendazole, thiophanate-methyl in concentrated juice by LC-MS/MS [J] Food Ind Sci Technol, 2012, 33(22): 56 59, 62. [14],,,. [J]., 2014, 24(10): Gou AH, Wang W, Zhao YY, et al. Determination of the residues of carbendazim in vegetables by HPLC [J]. Chin J Health Inspect, 2014, 24(10): [15]. [J]., 2004, 14(5): Hao JZ. Determination of carbendazim in fruits by HPLC [J]. Chin J Health Inspect, 2004, 14(5): 作者简介 ( 责任编辑 : 李振飞 ) 付艳梅, 本科, 助理工程师, 主要研究方向为食品理化检测 fuyanmei013@126.com 食品化学与营养专题征稿函, ; ; ; ;,,,,,,,,,,,,,,,, ,,, 投稿方式 : : jfoodsq@126.com 食品安全质量检测学报编辑部

g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min

g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min 25 4 2013 8 监测技术 5 1 2 1 ( 1. 江苏省疾病预防控制中心, 江苏南京 210009; 2. 南京医科大学第二附属医院, 江苏南京 210029) 5 Phenomenex kinetex C 18 2. 6 μm 4. 6 mm 150 mm 10 mmol /L ph 2. 5 + 60 40 DAD 280 nm 5 20. 0 mg /L ~ 100 mg /L 0.