Microsoft Word 冯晓青二校出1827

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1 7 5 Vol. 7 No Journal of Food Safety and Quality May, * 冯晓青, 汪怡, 王芹, 王露, 宋鑫, 杭学宇 (, ) 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 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 , 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 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 :,, @qq.com *Corresponding author: HANG Xue-Yu, Associate Chief Technician, Huai an Center for Disease Control and Prevention, No.118 Huaihai Road, Huai an , China @qq.com

2 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 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, 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 色谱条件优化流动相的选择 [17] -,, -, ( 30: 7040: 60 50: 50),,,, - 50: 50,, [18] 实验方法标准溶液配制 100 μl, 10 μg/ml, ng/ml, HPLC 样品前处理 1 10,,, 20, 1 Fig. 1 HPLC chromatogram of carbofuran standard 检测波长选择 2.2.3, 200~900 nm, 320 nm 285 nm 320 nm, 285nm 柱温的选择, 20 40,

3 5, : ,, 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,,, 线性关系及检测限 2.2.3,, 0.2~5.0μg/mL, ( 4), : Y=6.179X0.2884; r= S/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, 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(%) Fig. 5 (a) GPC (b) GPC Chromatograms of carbofuran spiked incelery samples (a) withoutgpc; (b) with GPC

4 结论,,,,, 参考文献 [1],,,. [J]. :, 2005, 41(4): Ji ZP, Wang SP, Lu ZQ, et al. Rapid determination of carbofuranbyspectrophotometry [J]. Phys Testing Chem Anal Part B: Chem Anal, 2005, 41(4): [2],,,. [J]., 2012, 51(2): GuoJ, Yang X, Zang C, et al. Exploring theestrogenicity of carbofuran and cypermethrin [J]. Agrochemicals, 2012, 51(2): [3] GB/TS [S] GB/TS Determination of plant foods in a variety of organophosphorus and carbamate pesticide residues [S]. [4],,,. 75 [J]., 2007, 17(8): Yang HC, Guo DH, Li B, et al. Determination of 75 pesticide in vegetable food by GPC-GC/MS [J]. ChinJ Health Lab Technol, 2007, 17(8): [5], 翀 [J]., 2014, 33: Che JS, Yu CT. A line gel chromatography GC-MS determination in vegetables 181 kinds of pesticide residues [J]. Chin J Anal Lab, 2014, 33: [6],,. 20 [J]. (), 2009, 27(1): Chen T, Shen SR, Yao YL. Determination of twenty pesticide residues in vegetable bygel permeation chromatography and solid phase extraction [J]. J Shanghai JiaotongUniv(AgricSci), 2009, 27(1): [7],,,. 77 [J]., 2007, 28(3): Wang MT, Mou J, Wu J, et al. Determination study of 77 organophosphrous and carbamate pesticide residue in fruits and vegetables [J]. Food Sci, 2007, 28(3): [8],,,. PSA 13 [J]., 2009, 28(11): Yu YB, Tan PG, Qu LL, et al. After phase extraction liquid chromatography column determination of vegetables and fruits 13 carbamate derivative fluorescence spectroscopy PSA dispersive solid [J]. Chin J Anal Lab, 2009, 28(11): [9],,,. SPE-GC/MS [J]., 2009, 35(2): Yang Y, Gao L, Jing L, et al. Study on method of organic phosphorus and carbamate pesticides in water using SPE and GC/MS [J]. China Meas, 2009, 35(2): [10],,,. [J]., 2003, 21(3): Liu CW, Liu XW, Zhai GS, et al. Determination of the multiresidue of carbamate insecticides and their metabolites in vegetables and fruits by solid-phase extraction and high performance liquid chromatography [J]. Chin J Chromatogr, 2003, 21(3): [11],,,. - N-[J]., 2006, 16(1): 911. Chen XH, Qiu PH, Jin MC, et al. Simultaneous determination of trace N-methycarbamates pesticides in water by solidphase extraction and HPLC with post-column derivatization [J]. Chin J Health Lab Technol, 2006, 16(1): 911. [12],,,. - 7 [J]., 2011, 32(6): Deng SG, Li ZM, Guo CY, et al. Determination of carbamate residues in vegetables by ultra-high performance liquid chromatography-tandemmass spectrometry [J]. Food Sci, 2011, 32(6): [13],. - [J]., 2007, 17(12): Cao YP, Wang DW. Determination of organophosphorus and carbamate pesticides in vegetables and fruits bygas chromatography-mass spectrometry and selected ion monitoring [J]. Chin J Health Lab Technol, 2007, 17(12): [14],,,. 40 [J]., 2007, 17(11): Zhao YH, He XF, Li Y, et al. A study on rapid determination of 40 organophosphorus and carbamate pesticide multi-residues in food [J]. Chin J Health Lab Technol, 2007, 17(11): [15],,, [J]., 2003, 22(6): Hu XZ, Chu XG, Yu JX, et al. Gas chromatography-mass spectrometry screening assays apple juice concentrate 105 kinds of pesticide residues [J]. J Instrum Anal, 2003, 22(6): [16] Wu G, BaoX, Zhao S, et al. Analysis of multi-pesticide residues in the foods of animal origin by GC MS coupled with accelerated solvent extraction and gel permeation chromatography cleanup [J]. Food Chem, 2011, 126(2): [17],,. / [J]., 2006, 18(1): Li J, Zhao YG, Yu JX, et al. Determination of carbamate pesticides in surfacewater using solidphase extraction and HPLC [J]. Adm Tech Environ Monit, 2006, 18(1): [18],,. -[J]. :, 2011, (4): Wang XN, Yan W, Liu Y. HPLC determination of carbofuran in water with pre-enrichment by SPE [J]. Phys Testing Chem Anal Part B: Chem Anal, 2011, (4): ( 责任编辑 : 姚菲 )

5 5, : 作者简介冯晓青, 技师, 主要研究方向为食品理化检验 [email protected] 杭学宇, 副主任技师, 主要研究方向为理化检验 @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

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