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1 4 6 Vol. 4 No Journal of Food Safety and Quality Dec., 魏欣欣 *, 窦彩云, 段永生, 马育松 (, ) 摘要 : 目的 - 方法,,, (trifluoroacetic anhtdride, TFAA) N- (1-methylimidazole, NMIM), C 18, 365 nm, 470 nm - 结果 10~500 ng/ml, r=0.999, 5 μg/kg %~103.1%, RSD 2.31%~6.93% 结论,, 关键词 : ; ; ; Determination of avermectin residues in dried chili by HPLC with fluorescence detection WEI Xin-Xin *, DOU Cai-Yun, DUAN Yong-Sheng, MA Yu-Song (Hebei Entry-Exit Inspection and Quarantine Bureau, Shijiazhuang , China) ABSTRACT: Objective To establish an HPLC with fluorescence dedection method for determination of avermectin residues in dried chili. Methods Residues are extracted with acetonitrile. The extract was cleaned up with acetonitrile saturated n-hexane and graphitized carbon solid-phase extraction cartridge. Avermectin residues were derived with trifluoroacetic acid and 1-methylimidazole and determined by reversed-phase liquid chromatography with fluorescence detection (excitation: 365 nm and emission: 470 nm). Results Recoveries ranged from 90.3% to 103.1% with RSD of % at spiking levels of 5, 10, 20 μg/kg. This method showed a good linearity over the range of 10~500 ng/ml with r= Conclusion This method is accurate, rapid, and highly sensitive and it is suitable for determination of avermectin residues in dried chili. KEY WORDS: avermectin; HPLC-FLD; dried chili; pesticide residues 1 引言 (avermectin, AVMs) Strptomyces avermitilis,, 20 ( 1),,, * 通讯作者 :,, CIQ_wxx@163.com *Corresponding author: WEI Xin-Xin, Assistant Engineer, Technical Center of Hebei Entry-Exit Inspection & Quarantine Bureau, No.318, Heping Road, Shijiazhuang CIQ_wxx@163.com

2 1842 4, [1-5],,,,, 2 材料与方法 2.1 仪器设备与试剂 : 1 Fig. 1 Molecular structure of avermectin (ng/kg ),,,, (World Health Organization, WHO)5 [6] AVMs, / (Food and Agriculture Organization/World Health Organization, FAO/WHO) (maximum residue limit, MRL) 0.01~0.02 mg/l [7], MRL 20 μg/kg [8] 2006 (positive system list) MRL, 10 μg/kg [9] [6-7] [8-12],,,,, [13], SN ,,,, [12],,, [10] - (LC-20AD, ); (PT3100, Kinmatic ); (4K-15, Sigma ); (Reacti-Therm III, Pierce ); (Vortex genie-2t, Scientific ); ( Agilent ); (Advantage A10+ELIX 5, Milli-Q ): (KQ-500E, ) (, Fisher ); (, ) ; + =3+1(v/v)(, ) ; Ⅰ: + =1+2(v/v)(,, Fluka ); Ⅱ: N- + =1+1(v/v)(N-,, Fluka ); (500 mg/6 ml ) ; ( 93.0%, Dr. Ehrenstorfer ) 2.2 色谱分析条件 : 150 mm 4.6 mm ODS C 18 ; : : 365 nm, : 470 nm; : : =94:6; : 1.5 ml/min; : 实验步骤样品制备,,,, 样品提取 2.5 g( 0.01 g) 50 ml, 10 ml, 20 min 1 min, r/min 10 min 样品净化, 10

3 6, : ml, 30 s,, 10 ml 500 mg, 5 ml + =3+1(v/v), 10 ml, 5 ml + =3+1(v/v), 0.5 ml/min 样品衍生化 50, 300 μl Ⅰ 200 μl Ⅱ, 15 min, 1 ml, HPLC-FLD ( ) 标准溶液配制 :, 100 μg/ml 4, 结果与分析 3.1 提取条件的选择,,,, [10],,,,,,,, [10],,,,,, 20% 30%, 20 min,,, 90% (solid-phase extraction, SPE) (immunoaffinity chromatography, IAC),,,, [9],,,, GPC, GPC,,, GPC, GPC [12] C 18 [12], C 18,,,, 90%, 3.3 衍生化条件的选择,,, N-, ( 2),,,, 15 min,, 15 min,, [13-14] 3.2 净化条件的选择, (liquid-liquid extraction, LLE) 2 Fig. 2 Derivatization reaction scheme

4 线性范围, 2.3.4, ng/ml,,, X, Y, Y=6758X+36859, r=0.999 ( 3, 4) 3.5 加标回收率的测定 μg/kg, ml 25 ng/ml,, 6, Fig.3 Standard curve of avermectin Fig.4 4 Chromatogram of avermectin standard 表 1 回收率和精密度 (n=6) Table 1 Recovery rate and precision(n=6) /(μg kg -1 ) /(μg kg -1 ) /(μg kg -1 ) /% RSD/%

5 6, : Fig. 5 Blank sample in dried chili 6 (5 μg/kg) Fig. 6 Spiked sample in dried chili (5 μg/kg), 5~20 μg/kg 3, 90.3%~103.1%, RSD 2.31%~ 6.93%, 4 结论,, ;, 5 μg/kg,, 参考文献 [1],,,. - [J]., 2009, 27(3): Yang F, Yang SS, Lin YH, et al. Determination of avermectin re-

1846 4 sidues in tea by ultra-performance liquid chromatography-electrospray tandem mass spectrometry [J]. Chin J Chromatogr, 2009, 27(3): 153 157. [2],,. [J]., 2009, 28(1): 84 88.

6 sidues in tea by ultra-performance liquid chromatography-electrospray tandem mass spectrometry [J]. Chin J Chromatogr, 2009, 27(3): [2],,. [J]., 2009, 28(1): Qin XG, Yuan KP, Ai XH. Determination of avermectin residues in aquatic products using HPLC with fluorescence detection [J]. J Huazhong Agric Univ, 2009, 28(1): [3]. [J]., 2012, 21(19): Li WP. Avermectin research [J]. Chin Pharm, 2012, 21(19): [4],,,. [J]., 2011, 39(8): Liang HF, Song J, Zhang WJ, et al. Study on the development method of avermectins residue in food determination [J]. J Shanxi Agric Sci, 2011, 39(8): [5] Virant Celestina T, Kolar L, Gobrc I, et al. Factors influencing dissipation of avermectins in sheep faeces [J]. Ecotox Environ Safe, 2010, 73(1): [6],. [J]., 2007, 31(4): Chen J, Luo YH. Progress in the research on the detection of avermetins residues in animal derived foods [J]. Guizhou Anim Sci Vet Med, 2007, 31(4): [7] Kolar L, Flajs VC, Kuzner J, et al. Time profile of abamectin and doramectin excretion and degradation in sheep faeces [J]. Environ Pollut, 2006, 144(1): [8],,,. 5 [J]., 2012, 31(10): Zhao XH, Cao ZY, Mou RX, et al. Determination of 5 avermectin residues in fruits and vegetables by liquid chromatography-tandem mass spectrometry [J]. J Instrum Anal, 2012, 31(10): [9] Seelanan P, Srisa-Art M, Petsom A, et al. Determination of avermectins in commercial formulations using microemulsion electrokinetic chromatography [J]. Anal Chim Acta, 2006, 570(1): [10],,. [J]., 2010, 43(16): Zhao Y, Xie XC, Zhan XP. Multi-residues determination of abamectin, emamectin benzoate and ivermectin in vegetables by HPLC-FD [J]. Chin Sci Agric, 2010, 43(16): [11] Cobin JA, Johnson NA. Liquid chromatographic method for rapid determination of total avermectin B1 and 8, 9-Z-avermectin B1 residues in apples [J]. J AOAC Int, 1995, 78(2): [12]. [J]., 2006, 5(6): Ma YS. Determination of abamectin residues in fruits by high-performance liquid chromatography with fluorescence detection [J]. Mod Agrochem, 2006, 5(6): [13] SN/T [S]. SN/T Determination of abamectin residues in fruit vegetable for import and export-lc method [S]. [14],,,. [J]., 2012, 3: Luo CY, Cha YB, Ren JH, et al. Determination of avermectins residues in plant derived food by HPLC [J]. Anal Instrum, 2012, 3: 作者简介 ( 责任编辑 : 赵静 ) 魏欣欣, 本科, 助理工程师, 主要研究方向食品安全检测技术 CIQ_wxx@163.com

Microsoft Word _刘丽丽-二校

Microsoft Word _刘丽丽-二校 7 2 Vol. 7 No. 2 2016 2 Journal of Food Safety and Quality Feb., 2016 刘丽丽 *, 刘谦, 王宇 (, 071001) 摘要 : 目的, 方法, HLB, C 18, ESI 结果 0.1~10 μg/kg, 0.999, 0.1 0.2 10.0 μg/kg 3, 95.0%~103.2%, 3.72%~6.85%, 0.1