6 8 Vol. 6 No. 8 2015 8 Journal of Food Safety and Quality Aug., 2015 付艳梅 *, 王海霞, 张秀丰 (, 053000) 摘要 : 目的 方法 1% -, MCX,, C 18, -, 274 nm, 结果 0.10 4.0 mg/l,, 0.9998, 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 053000, 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 0.9998, and the detection limit was 0.020 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 :,, E-mail: fuyanmei013@126.com *Corresponding author: FU Yan-Mei, Assistant Engineer, Hengshui Entry-Exit Inspection and Quarantine Bureau, No. 1396, Renmin Road, Hengshui 053000, China. E-mail: fuyanmei013@126.com
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 0.1 0.5 1 2 4 µg/ml 2.4 样品前处理 2.4.1 样品的制备,, 4 2.4.2 样品提取 10 g ( 0.01 g) 50 ml, 40 ml 1% - 1 min, 4000 r/min 5 min, 2.4.3 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 3.1.1 溶剂的选择,,,,, 1% - 1% -, 1% -,, 60%, 1% -, 85%, 1% - [14] 3.1.2 净化方法的选择, Oasis MCX [15] 3 ml 1% -,, 3.1.3 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 2 80 0.10~4.0 mg/l,, Y=28266X-30, r 2 =0.9998. 3 (S/N=3), 0.02 mg/kg 1 3.3 回收率与精密度 10 g, 0.1 1.0 2.0 mg/kg 3, 1, 2, 3
3280 6 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
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3282 6 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): 1407 1410. 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): 1407 1410. [15]. [J]., 2004, 14(5): 586 587. Hao JZ. Determination of carbendazim in fruits by HPLC [J]. Chin J Health Inspect, 2004, 14(5): 586 587. 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 E-mail: fuyanmei013@126.com 食品化学与营养 专题征稿函, ; ; ; ;,,,,,,,,,,,,,,,, 2015 11,,, 2015 10 10 E-mail 投稿方式 : : www.chinafoodj.com E-mail: jfoodsq@126.com 食品安全质量检测学报 编辑部