7 4 Vol. 7 No. 4 2016 4 Journal of Food Safety and Quality Apr., 2016 6 周红英 *, 房信胜, 刘静, 李坤, 郝丽君 (, 271018) 摘要 : 目的 6 方法 3 min 50, Carb/PSA, ( FPD ) 结果 6 μg/ml, r>0.997, 78.5%~94.3%, RSD 1.7%~5.9%, 0.53~1.16 μg/kg 3 6 结论 3 min 50 3 关键词 : ; ; Effects of different drying processes on 6 kinds of organophosphate pesticide residues in chrysanthemum ZHOU HongYing *, FANG XinSheng, LIU Jing, LI Kun, HAO LiJun (College of Agronomy, Shandong Agricultural University, Taian 271018, China) ABSTRACT: Objective To study the effects of different drying processes on 6 kinds of organophosphate pesticide residues including oxygen dimethoate, dichlorvos, methyl parathion, phorate, phosphorus absorption and parathion in Chrysanthemum morifolium. Methods Chrysanthemum polluted by organophosphate pesticides were processed by airdrying after steaming 3 min, 50 heatdrying, airdrying and drying, respectively, then extracted with acetonitrile, purified by Carb/PSA solid phase extraction, and detected by gas chromatography (GC, equipped with FPD detector). Results Six kinds of organophosphate pesticides had good linear relationships in the range of μg/ml with the correlation coefficients r>0.997, the recoveries were in the range of 78.5%~94.3%, RSDs were in the range of 1.7%~5.9%, and the limits of quantitation were ranged from 0.53 to 1.16 μg/kg. Six kinds of organophosphate pesticides had not been detected in the 3 kinds of dried chrysanthemums. Conclusions Three kinds of drying methods can significantly reduce the organophosphate pesticide residues in chrysanthemum. KEY WORDS: chrysanthemum; drying method; organophosphate pesticide 基金项目 : (20123069) Fund: Supported by the Science and Technology Project of Taian (20123069) * 通讯作者 :,, Email: zhouhy@sdau.edu.cn *Corresponding author: ZHOU HongYing, Associate professor, College of Agronomy, Shandong Agricultural University, Taian 271018, China. Email: zhouhy@sdau.edu.cn
4, : 6 1701 1 引言,, [18] [913] (Chrysanthemum morifolium Ramat.),,,,,,,, (2015 ) [14] ( ),,, 2 材料与方法 2.1 仪器与试剂 GC2010 ( FPD, ); LXJIIB (); KQ5200E ( ); N1000 ( ) (, ); (, ); Carb/PSA (500 mg/6 ml, DIKMA ); MilliQ (MC GBW(E) 081328) (MC GBW(E) 081320)(MC GBW(E) 081324) (MC GBW(E) 081321) (MC GBW(E) 081357) (MC GBW(E) 081323) 1000 mg/l, ( ) 2.2 材料, (Chrysanthemum morifolium Ramat.), 200 g 2 μg/ml 24 h,, :. (1) : 50 g,, (25 ) 4~5 d, (2) 3 min :, 50 g,, 3 min,, (25 ) 4~5 d, (3)50 : 50 g,, 50 1~2 d, (4) : 50 g,, (25 ), 2.3 实验方法 2.3.1 标准溶液的制备 6 0.2 ml, 100 ml,, 2 μg/ml, 0 0.01 0.02 0.04 0.08 μg/ml, 2.3.2 提取和净化 (1) 2.0 g, 50 ml, 30 ml,,, 30 min, 3500 r/min 5 min, 35, (2) Carb/PSA 0.5 g, 4 ml ( 3: 1) 10 ml 3,, 20 ml,, 35 0.5 ml, 1 ml, 0.22 μm, 2.3.3 气相色谱条件 : HP1701(30 m 0.32 mm, 0.25 μm ); : 250 ; : 260 ; : 160 (2 min), 10 /min 200, 4 min, 2 /min 250 ; ( ) : 3 ml/min; ( ): 5 μl 3 结果与分析 3.1 分析条件的选择 3.1.1 前处理方法的选择, 1% (1:2, V:V) [1517] 4,
1702 7,,, Carb/PSA,,,,,, 3.1.2 色谱条件的选择 2005 2010, 2015,, [15,17], FPD, 20 min 6,, 6 1 3.1.3 线性关系 0 0.01 0.02 0.04 0.08 μg/ml, 2.3.3,,,,,, 1 3(S/N=3) (LOD), 6 1 3.1.4 精密度和回收率, 6 5 10 20 μg/kg 3, 5,,, 2 2, 6 83.2%~86.9%, 2.2%~4.6%, 1 6 GC Fig. 1 GC chromatogram of 6 kinds of organophosphate pesticides : 1.; 2.; 3.; 4.; 5. ; 6. Note: 1.dichlorvos; 2.demeton; 3.phorate; 4.omethoate; 5.parathionmethyl; 6. parathionethyl. 3.2 干燥方法的选择 45~50 ; 3~5 min ;,, 3 min 50 3 3.3 样品测定, 2.3.3, 3.1.3, 1 kg 500 ml 6, 3,, 3 min 50 6,, 6 Table 1 表 1 6 种有机磷农药的线性方程和检出限 Linear equations and LODs of 6 kinds of organophosphate pesticides r (μg /ml) (μg / kg) (min) Y=977112X168773 0.9983 0.74 2.53 Y=25636X+766.05 0.9996 1.16 5.45 Y=475320X+26031 0.9971 0.53 6.62 Y=232644X+19809 0.9995 0.84 7.72 Y=311649X7655.4 0.9998 0.68 12.60 Y=282426X+9098.5 0.9998 0.61 14.68
4, : 6 1703 Table 2 表 2 6 种有机磷农药在 3 种加标水平下的回收率及相对标准偏差 (n=5) Spiked recoveries and RSDs of 6 kinds of organophosphate pesticides spiked at 3 levels (n=5) (μg/kg) 5 10 20 (%) (%) (%) (%) (%) (%) 84.6 2.2 90.3 2.6 78.5 1.7 85.7 5.9 79.7 2.8 84.7 4.6 89.5 4.3 79.8 5.5 85.8 3.5 79.4 4.2 81.4 3.4 91.9 3.3 90.1 5.3 85.4 3.9 83.2 4.6 94.3 5.4 79.8 4.1 86.6 3.9 Table 3 表 3 不同干燥方法处理后的菊花中 6 种有机磷农药残留量结果 (n=3) Results of 6 kinds of organophosphate pesticide residues in chrysanthemum processed by different drying methods(n=3) (μg/kg) (μg/kg) (μg/kg) (μg/kg) (μg/kg) (μg/kg) 3 min 50 ( ) 9.42 12.08 11.46 11.24 15.56 13.06 : 4 结论 6, 3 min 50 3, 6 参考文献 [1],,,. 33 [J]., 2011, 23(4): 330 335. Yu H, Chen A, Li XJ, et al. Determination of 33 organophosphorous pesticide residues in vegetables by GCSPE [J]. Chin J Food Hyg, 2011, 23(4): 330 335. [2] Ji J, Deng C, Zhang H, et al. Microwaveassisted stean distillation for the determination of organochlorine pesticides and pyrethroids in Chinese teas [J]. Talanta, 2007, 71(3): 1068 1074. [3] Li Y, Chen X, Fan C, et al. Compensation for matrix effects in the gas chromatographymass spectrometry analysis of 186 pesticides in tea matrices using analyte protectants [J]. J Chromatogr A, 2012, 1266: 131 142. [4],,. [J]., 2015, 6(9): 3746 3751. Zhu CY, Xv ML, Liu JB. Determination of dichlorvos and malathion in corn beverage by gas chromatographymass spectrometry [J]. J Food Saf Qual, 2015, 6(9): 3746 3751. [5],,,. [J]., 2015, 6(5): 1743 1747. Yi DW, Zou Y, Liu Y, et al. Evaluation of uncertainty for diazinon residues in Astragali radix by gas chromatographymass spectrometry method [J]. J Food Saf Qual, 2015, 6(5): 1743 1747. [6] Sinha SU, Rao MVV, Vasudev K, et al. A liquid chromatography mass spectrometrybased method to measure organophosphorous insecticide, herbicide and non organophosphorous pesticide in grape and apple samples [J]. Food Control, 2012, 25: 636 646. [7],,. 18 [J]., 2006, 31(16): 1321 1323. Xiang ZX, Zhao WJ, Guo QS. Determination of 18 organophosphate pesticide residues in Flos lonicerae [J]. China J Chin Mater Med, 2006, 31(16): 1321 1323. [8],,,. 12 [J]., 2007, 7(2): 115 118.
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