5种农药在采收前和初烤后的烟叶及土壤中的残留量变化-烟草科技.PDF

2016 年7 月 烟草科技 Jul. 2016 第49 卷第7 期 Tobacco Science Technology Vol. 49 No. 7 55 种农药在采收前和初烤后的烟叶及土壤中的 残留量变化 司晓喜，刘志华，李中昌，张凤梅，陆舍铭，尤俊衡，刘春波，沈艳飞，朱瑞芝* 云南省烟草化学重点实验室，云南中烟工业有限责任公司技术中心，昆明市五华区红锦路367 号 650231 摘要：为研究采收前和初烤后烟叶及土壤中三唑酮、霜霉威、稻瘟灵、吡虫啉和仲丁灵残留量的变化，建 立了烟叶和土壤中该5 种农药残留的超高效液相色谱- 串联质谱（UPLC-MS/MS ）分析方法。样品经乙 腈提取，N- 丙基乙二胺（PSA ）吸附剂净化，UPLC-MS/MS 法检测，采用基质配制溶液绘制标准曲线，内 标法定量。结果表明：①烟叶中5 种农残的定量限在12.25~37.48 μg/kg 之间，加标回收率为74%~ 117% ； 土壤中5 种农残的定量限在0.11~0.34 μg/kg 之间，加标回收率为78%~ 107% 。②田间试验表明，于烟叶 采收前15 d 对烟草植株按最大许可使用量施药后，上部、中部叶中吡虫啉、三唑酮（含其残留的转化物三 唑醇）和仲丁灵的残留量随时间逐渐减小；霜霉威和稻瘟灵的残留量随时间先增大后减小；初烤后烟叶 中5 种农药的最终残留量≤2.70 mg/kg ，低于CORESTA 规定的指导性残留限量（GRLs ）。土壤中吡虫啉 残留量随时间逐渐减小；三唑酮、稻瘟灵和霜霉威的残留量随时间先增大后减小；仲丁灵残留量随时间 有所增加。 关键词：烟叶；土壤；农药残留量；超高效液相色谱- 串联质谱法（UPLC-MS/MS ） 中图分类号：TS411 ；S482 文献标志码：A 文章编号：1002-0861 （2016 ）07-0044-07 Residuesoffivepesticidesin tobaccoleavesbeforeharvestingandafterflue-curing andsoils SI Xiaoxi, LIU Zhihua, LI Zhongchang, ZHANG Fengmei, LU Sheming, YOU Junheng, LIU Chunbo, SHEN Yanfei, ZHU Ruizhi* Key Laboratory of Tobacco Chemistry of Yunnan, RD Center of China Tobacco Yunnan Industrial Co., Ltd., Kunming 650231, China Abstract: In order to study the variations of five pesticide residues in tobacco leaves before harvesting and after flue-curing and soils, an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the quantification of the residues in test samples. Samples were extracted with acetonitrile and cleaned up by primary secondary amine (PSA) sorbent, then detected by UPLC-MS/MS. Quantitative methods were established using matrix-matched calibration standards and internal standards. The results showed that: 1) For tobacco samples, the limits of quantification (LOQs) ranged from 12.25 to 37.48 μg/kg and the recoverie