Microsoft Word 李增梅-二校出1001，1002,1003

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1 6 3 Vol. 6 No Journal of Food Safety and Quality Mar., 2015 李增梅, 邓立刚 *, 赵善仓, 张树秋, 郭长英, 梁京芸, 董燕婕 (,, ) 摘要 : 目的,, (HPLC), 方法 / (v:v, 60:40), PCX, Waters Atlantis C 18 (3.6 mm 250 mm, 5 µm) 结果 (LOQ) 0.01 mg/kg; 0.02~10 µg/ml, R= %~94.5%, RSD 2.9%~6.5%, 2.8~5.1, 2.1~4.3 ;, 结论,, 关键词 : ; ; ; ; Residue decline study of nitenpyram in cotton and soil LI Zeng-Mei, DENG Li-Gang *, ZHAO Shan-Cang, ZHANG Shu-Qiu, GUO Chang-Ying, LIANG Jing-Yun, DONG Yan-Jie (Key Laboratory of Test Technology on Food Quality and Safety of Shandong Province, Institute of Agricultural Quality Standards and Testing Technology Research, Shandong Academy of Agricultural Sciences, Jinan , China) ABSTRACT: Objective To establish a method for the determination of nitenpyram in cotton leaves and soil by high performance liquid chromatography (HPLC). Degradation of nitenpyramin cotton and soil using this HPLC method was studied. Methods Samples were extracted by methanol/water (60:40, v:v), and then purified by PCX extraction column. The analysis were separated on a Waters Atlantis C 18 (3.6 mm 250 mm, 5 µm)and detected by HPLC. Results This method provided a high linearity of the working curve for calibration as well as repeatability and reproducibility. The limits of quantification (LOQ) were 0.01 mg/kg in cotton and soil. The correlation coefficient of the working curve for calibration was for the nitenpyram in the concentration range from 0.02 to 10 µg/ml. The recoveries of nitenpyram in cotton, seed and soil were 71.5%~94.5%, and RSD were 2.9%~6.5%. The results showed the half-lives of nitenpyram were 2.8~5.1 d at cotton, and 2.1~4.3 d in soil. The final residues of nitenpyram were undetectable. Conclusion The method is simple and accurate for the determination of nitenpyram. Nitenpyram was an easily degradable insecticide. KEY WORDS: high performance liquid chromatography; nitenpyram; cotton; soil; residues * 通讯作者 :,, deng_ligang@163.com *Corresponding author: DENG Li-Gang, Research Associate, Institute of Agricultural Quality Standards and Testing Technology Research, Shandong Academy of Agricultural Sciences, Jinan , China. deng_ligang@163.com

2 3, : 引言 (nitenpyram),,,, [1-4] [5,6],, [7], [8] MRL, 0.05 mg/kg, 0.5 mg/kg; 0.03 mg/kg, 0.5 mg/kg [9,10], [11-14] [14,15], [12] -; [13],,,,,,, [12],,, ; [7],,,,,,,, 2 材料与方法 2.1 仪器设备 Waters (2695, Waters ), (2487, Waters ); (IKA-WERLE T25BS2, IKA ); Heidolph (L4000, Heidolph ); (3K30, Sigma ); (KQ-500E, ); (IKA-MS3, IKA ); (SE202F, ); (10~100 µl, 100~1000 µl, Eppendorf ) (OA-SYS, Organomation ) 2.2 试剂 (>99%, Sigma ); (, Sigma ); (, ); (, ); (, ) 2.3 田间试验试验设计, 30 m 2, 3,,, 67.5 g/hm 2 (), 45 g/hm 2 ( ),, 消解动态试验,, 1, 2 h d, : 500 g, 25 ; : 0~10 cm 1 kg, 1 mm, 最终残留试验 2,, 2 3,, d :, 1 kg,,, 25 : 0~15 cm 1 kg, 1 mm, 分析方法标准溶液的配制 10.0 mg 100 ml

3 1002 6,, µg/ml; 10.0 µg/ml, µg/ml, 样品制备 : 5.0 g( 5.0 g), 25 ml ; (v:v, 60:40), 10 ml, PCX : 10.0 g, 25 ml, 净化 PCX(60 mg, 3 ml) 5 ml, 5 ml,, 3 ml, 10 ml, 3 ml (5%),, ; (v:v, 20:80)( 1 ml, 2 ml), 添加回收试验 mg/kg 3, 分析条件 : Atlantis C 18 (3.6 mm 250 mm, 5 µm); : 30 ; : :(90:10); : 1.0 ml/min; : 260 nm; : 10 µl 15.0 min 结果计算,,, : Cst Pi Vsti V R m Vi Psti : R: (mg/kg); Cst: (µg/ml); V sti : (µl); Pi: ; V: (ml); Vi: (µl); Psti: ; m: (g) 3 结果与分析 3.1 方法灵敏度准确度和精密度 0.02~10 µg/ml, 10 µl 0.1~10 µg/ml, Y (µv*sec) X (µg/g) ( 1, A), Y=2370.5X , R mg/kg, (0.05 mg/kg),, 71.5%~93%, 76.5%~93.3%, 77.5%~94.5%, ( RSD ) 2.9% 6.5%, ( 1, B~K) 3.2 净化方法优化,,, PSA MgSO 4,,, PCX,,,, 3.3 烯啶虫胺在棉叶和土壤中的消解动态 1, 10 d, %, >90%,, C=C 0 e -kt ( 1) d 2.8 d, 2.9 d 2.9 d, 4.3 d 2.7 d, 4.4 d 2.1 d 3.4 烯啶虫胺在棉籽和土壤中的最终残留 ( 2),, (0.01 mg/kg):, ; ;,,,,

4 3, : HPLC Fig. 1 Chromatograms of blank sample and samples spiked with nitenpyram A: ; B: (1.0 μg/ml); C: ; D: (0.1 mg/kg); E: ; F: ; G: (0.1 mg/kg); H: ; I: ; J: (0.1 mg/kg); K: A: standard curve; B: nitenpyram standard spectrum (1.0 μg/ml); C: soil blank spectrum; D:soils map (0.1mg/kg); E: soil sample spectrum; F: cotton leaf blank spectrum; G: cotton leaves add maps (0.1mg/kg); H: cotton leaf sample spectrum; I: cottonseed blank spectrum; J: cottonseed adding spectrum (0.1 mg/kg); K: cottonseed sample spectrum.

5 Table 1 表 1 烯啶虫胺在棉叶和土壤中的消解代谢规律 Dynamic degradation equation of nitenpyram in cotton leaves and soil (mg/kg) 1 (R) (d) (mg/kg) 1 (R) (d) C=2.1529e t C=0.4551e t C= e t C=0.4161e t C= e t C= e t C= e t C=0.4098e t ) C t =C 0 e -kt, C t : t, mg/kg; C 0 : mg/kg; : ; t:, d Table 2 表 2 烯啶虫胺在棉叶棉籽和土壤中的添加回收率 (n=5) The recoveries of nitenpyram in cotton, soil and cotton seed (n=5) (mg/kg) (%) (%) RSD(%) 参考文献 [1]. [J]., 2011(3): Cao DH. Nitenpyram [J]. Hunan Agric, 2011(3): [2],. [J]., 2009(11): Sun H, Yang CH. New insecticides Nitenpyram [J]. Fine Specialty Chem, 2009(11): [3],,,. [J]., 2012, 16(2): 1 5. Li M, Cheng SX, Li HP, et al. Neonicotinoids nitenpyram review [J]. Agrochem Res Appl, 2012, 16(2): 1 5. [4]. [J]., 2010, 34: 018. Wang X. New pesticides-nitenpyram [J]. Agr Knowl, 2010, 34: 018. [5],,,. [J]., 2010, 22(9): Shu ZL, Sun TD, Zhang F, et al. Control effect of nitenpyram against nilaparvata lugens in rice field [J]. Jiangxi J Agr Sci, 2010, 22 (9): [6],,,. [J]., 2011, 42(8): Ling Y, Zhong Y, Wei SD, et al. Toxicity of nitenpyram, ethofenprox and their mixtures on nilaparvatalugens [J]. J South Agric, 2011, 42(8): [7],,. 10% 60% [J]., 2014, 35(1): Tang XL, Chen WG, Sun HY. 10% Nitenpyram agent and 60% nitenpyram wettable powder toxicity determination under silkworm acute food [J]. China Sericult, 2014, 35(1): [8],,,. 3 [J]., 2010, 49(1): Xie HP, Song QA, Jin LH, et al. Toxicity measure of buprofezin,

3, : 1005 nitenpyram and their mixtures to the third instar nymphs of brownplant hopper [J]. Agrochemica, 2010, 49(1): 74 77. [9] GB 2763-2014 [S].

Pesticide residues in agricultural products monitored in Hyogo Prefecture, Japan, FYs 1995 1999 [J]. J AOAC Int, 2002, 85(3): 692 703. [11],,,. [J]., 2012, 14(4): 423 428 Fu Y, Lin T, Chen ML, et al.

6 3, : 1005 nitenpyram and their mixtures to the third instar nymphs of brownplant hopper [J]. Agrochemica, 2010, 49(1): [9] GB [S]. GB National food safety standard-maximum residue limits for pesticides in food [S]. [10] Akiyama Y, Yoshioka N, Tsuji M. Pesticide residues in agricultural products monitored in Hyogo Prefecture, Japan, FYs [J]. J AOAC Int, 2002, 85(3): [11],,,. [J]., 2012, 14(4): Fu Y, Lin T, Chen ML, et al. Residues decline study of nitenpyram in orangeand soil [J]. Chin J Pestic Sci, 2012, 14(4): [12],,,. [J]., 2010, 29(4): Lu CH, Liu XG, Dong FS, et al. Residueand degradation of nitenpyramin cotton and soil [J]. Environ Chem, 2010, 29(4): [13],,,. [J]., 2012, 14(5): Yang JC, Hu DY, Zhang YP, et al. Residueand decline of nitenpyramin rice and riec field [J]. Chin J Pestic Sci, 2012, 14(5): [14],,,. - [J]., 2013, 36(6): Wang FR, Zhang JJ, Wu P, et al. Determination method of buprofezin and nitenpyram residues in rice field [J]. J Nanjing Agric Univ, 2013, 36(6): [15],,,. [J]., 2010, 28(11): Zhang GQ, Nie SQ, Long LP, et al. Determination of nitenpyram residue in cabbage and soil using gas chromatography [J]. Chin J Chromatogr, 2010, 28(11): 作者简介 ( 责任编辑 : 张宏梁 ) 李增梅, 博士, 副研究员, 主要研究方向为食品质量与安全检测技术邓立刚, 副研究员, 主要研究方向为食品质量与安全检测技术 deng_ligang@163.com

g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min

g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min 25 4 2013 8 监测技术 5 1 2 1 ( 1. 江苏省疾病预防控制中心, 江苏南京 210009; 2. 南京医科大学第二附属医院, 江苏南京 210029) 5 Phenomenex kinetex C 18 2. 6 μm 4. 6 mm 150 mm 10 mmol /L ph 2. 5 + 60 40 DAD 280 nm 5 20. 0 mg /L ~ 100 mg /L 0.

Microsoft Word 李增梅-二校 出1001，1002,1003

Microsoft Word 李增梅-二校出1001，1002,1003