7 5 Vol. 7 No. 5 2016 5 Journal of Food Safety and Quality May, 2016 - * 冯晓青, 汪怡, 王芹, 王露, 宋鑫, 杭学宇 (, 223001) 摘要 : 目的 - 方法 -, C 18,, 285 nm, 320 nm, 结果 0.2~5.0 ng/ml, r 0.999, 0.01 mg/kg 3 0.51.0 2.0 mg/kg, 78.3%~97.6%, 3.26%~11.69% 结论, 关键词 : ; ; ; Determination of carbofuran in vegetables by gel permeation chromatography-highperformance liquid chromatography FENG Xiao-Qing, WANG Yi, WANG Qin, WANG Lu, SONG Xin, HANG Xue-Yu * (Huai an Center for Disease Control and Prevention, Huai an 223001, China) ABSTRACT: Objective To establish a method for determination of carbofuraninvegetablesby high performance liquid chromatography (HPLC) with purification ofgel permeation chromatography (GPC). Methods Samples were extracted withacetonitrile and dissolved with ethyl acetate-cyclohexanemixture, and then separated by reversed-phase C 18 column followed with GPC purification.the fluorescence excitation and emission wavelengths were 285 nm and 320 nm. Identification of carbofuran was performed by HPLC with an external standard method. Results Carbofuranhad a good linear relationship in the range of 0.2~5.0 ng/ml with the correlation coefficient greater than 0.999. The limit of detection(lod) was0.01mg/kg. The average recoveries at 3 spiked levels of 0.5, 1.0 and 2.0 mg/kg were ranged from 78.3% to 97.6%, and the relative standard deviations(rsd)were in the range of 3.26%~11.69%. Conclusion The established method is simple and sensitive, which issuitable forthe determination of carbofuran in vegetables. KEY WORDS: high performance liquid chromatography;carbofuran;gelpermeation chromatography; vegetables 1 引言,, [1,2],, * 通讯作者 :,, E-mail: 664686545@qq.com *Corresponding author: HANG Xue-Yu, Associate Chief Technician, Huai an Center for Disease Control and Prevention, No.118 Huaihai Road, Huai an 223001, China. E-mail: 664686545@qq.com
1828 7,, [3], (gel permeation chromatography, GPC) [4-6] (solid phase extraction, SPE) [7-11] - [12-14] [15] GPC,, GPC - GPC -(gas chromatography-mass spectrometry, GC-MS), GPC, [16] 10, GPC (HPLC),, 2 材料与方法 2.1 仪器与试剂 HPLC-1260 ( ); PrepLinc Platform ( J2 Scientific ); DB-3D ( Techene ); LABOROTA 4000 ( Heidolph ); SI-0256 ( Scientific Industries ); OK1082A () : 100 μg/ml, (, Merck ); (, ); (, ); 0.22 μm (); Millipore 2 25 g( 0.01 g), 50 ml, 2 min 5~7 g, 40~50 ml, l min, 10 min, 10mL 80 10 ml -(50:50, V:V),, GPC 3 GPC -(50:50, V:V), 4.6mL/min, 10~20 min GPC, 2.0 ml -(1:1, V:V),, 0.22 μm, 2.2.3 仪器条件 : : Agilent TC-C 18 (4.6 mm 25 cm, 5 μm); : 35 ; : 285 nm, 320 nm; : -(1: 1, V: V) 3 结果与分析 3.1 色谱条件优化 3.1.1 流动相的选择 [17] -,, -, ( 30: 7040: 60 50: 50),,,, - 50: 50,, [18] 1 2.2 实验方法 2.2.1 标准溶液配制 100 μl, 10 μg/ml, 20 0.20.51.02.0 5.0 ng/ml, HPLC 2.2.2 样品前处理 1 10,,, 20, 1 Fig. 1 HPLC chromatogram of carbofuran standard 3.1.2 检测波长选择 2.2.3, 200~900 nm, 320 nm 285 nm 320 nm, 285nm 3.1.3 柱温的选择, 20 40,
5, : - 1829,, 35 3.2 GPC 条件优化 GPC, Bio-Beads S-X3(300 mm 10 mm)-(1:1, V:V), 4.6 ml/min, GPC ( 2), 9~13 min,, GPC,,, 3 3.3 线性关系及检测限 2.2.3,, 0.2~5.0μg/mL, ( 4), : Y=6.179X0.2884; r=0.9993 3S/N 0.01 mg/kg 4 Fig. 4 Standard curve of carbofuran Fig. 2 2 GPC The eluting chromatogram of carbofuranby GPC 3.4 仪器精密度实验 5.0 μg/ml, 6, RSD 0.108% 3.5 稳定性实验 5.0 µg/ml, 2 h, 10 µl, 30.81, RSD 0.131%: 12 h 3.6 重复性实验 6, 2.2.2, 2.2.3, 1.78 μg/kg, RSD 1.58% 3.7 方法回收率实验, 1 0.501.002.00 μg/kg, 78.3%~97.6%, RSD 3.26%~11.69% 表 1 空白样品中呋喃丹的加标回收率 精密度 (n=3) Table 1 Recoveries and RSD at 3 spiked levels for carbofuran in blank sample (n=3) (μg/kg) (μg/kg) (%) RSD(%) 3 0.50 78.3 3.26 Fig. 5 (a) GPC (b) GPC Chromatograms of carbofuran spiked incelery samples (a) withoutgpc; (b) with GPC. 0 1.00 80.7. 11.69 2.00 97.6 8.77
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5, : - 1831 作者简介 冯晓青, 技师, 主要研究方向为食品理化检验 E-mail: fengxiaoqing-20@163.com 杭学宇, 副主任技师, 主要研究方向为理化检验 E-mail: 664686545@qq.com 功能性食品微生物 专题征稿函 投稿方式 : 食品安全质量检测学报 编辑部