| 韩慧鸾1, 2, 张笑中2, 董丰收2*, 徐 军2, 吴小虎2, 潘兴鲁2, 郑永权2.超高效液相色谱-串联质谱同时检测甘蔗及土壤中5种农药残留[J].植物保护,2025,51(3):282-288. |
| 超高效液相色谱-串联质谱同时检测甘蔗及土壤中5种农药残留 |
| Determination of five pesticide residues in sugarcane and soil by ultra-high performance liquid chromatography-tandem mass spectrometry |
| 投稿时间：2024-06-23 修订日期：2024-08-10 |
| DOI：10.16688/j.zwbh.2024338 |
| 中文关键词: 超高效液相色谱-串联质谱 甘蔗 土壤 农药残留 杀虫剂 |
| 英文关键词:UPLC-MS/MS sugarcane soil pesticide residues insecticides |
| 基金项目:国家自然科学基金(32472620) |
| 作者 | 单位 | E-mail | | 韩慧鸾1, 2, 张笑中2, 董丰收2*, 徐 军2, 吴小虎2, 潘兴鲁2, 郑永权2 | 1. 海南大学热带农林学院, 海口 570228
2. 中国农业科学院植物保护研究所, 植物病虫害综合治理全国重点实验室, 北京 100193 | dongfengshou@caas.cn |
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| 中文摘要: |
| 本研究建立了QuEChERS-超高效液相色谱-串联质谱(QuEChERS-UPLC-MS/MS)同时检测甘蔗及土壤中噻虫嗪、噻虫胺、毒死蜱、吡虫啉及氯虫苯甲酰胺的农药残留分析方法, 为监测甘蔗生产中的农药应用风险提供方法参考。甘蔗和土壤样品分别经0.1%甲酸-乙腈和乙腈振荡提取后, 采用QuEChERS方法净化, 流动相为甲醇和0.2%甲酸水, 采用C18色谱柱进行分离, 基质匹配标准曲线外标法定量分析。结果表明:在0.01、0.1 mg/kg和1 mg/kg 3个添加水平下, 目标化合物的平均回收率为81.9%~115.5%, 相对标准偏差(relative standard deviations, RSD)为1.3%~11.8%, 该方法在0.01~1 mg/kg范围内线性良好, 决定系数R2≥0.990 0, 定量限(limits of quantification, LOQ)为0.01 mg/kg。该方法准确、快速、灵敏度高, 可满足甘蔗和土壤中噻虫嗪、噻虫胺、毒死蜱、吡虫啉及氯虫苯甲酰胺的检测方法要求。利用该方法对广西某产区的甘蔗农药残留进行监测, 发现少量甘蔗样品中噻虫胺残留超标, 其他目标杀虫剂在甘蔗样品中农药残留量符合农药限量安全标准。 |
| 英文摘要: |
| In this study, an analytical method for the simultaneous determination of pesticide residues of thiamethoxam, clothianidin, chlorpyrifos, imidacloprid and chlorantraniliprole in sugarcane and soil by QuEChERS-ultra-high liquid chromatography-tandem mass spectrometry (QuEChERS-UPLC-MS/MS) was established for monitoring the risk of pesticide application in sugarcane production. The sugarcane and soil samples were extracted by 0.1% formic acid-acetonitrile and acetonitrile, respectively, and then cleaned up by the QuEChERS method with the mobile phases of methanol and water containing 0.2% formic acid. The separation was carried out on a C18 column, and the quantitative analysis was performed by the external standard method with matrix-matched standard curve. The results showed that the mean recoveries of the target compounds ranged from 81.9% to 115.5%, with relative standard deviations of (RSD) 1.3% to 11.8% at the three spiked levels of 0.01, 0.1 mg/kg and 1 mg/kg, and the method showed good linearity in the range of 0.01 mg/kg to 1 mg/kg with the correlation coefficients all higher than 0.990 0. The limits of quantification (LOQs) of the method were 0.01 mg/kg. The method is accurate, fast and sensitive and can meet the requirements for the determination of thiamethoxam, clothianidin, chlorpyrifos, imidacloprid and chlorantraniliprole in sugarcane and soil. The method was used to monitor pesticide residues in sugarcane collected from Guangxi, finding that clothianidin in some samples exceeded the standard, while the other targeted pesticides residues in sugarcane samples met the safety standards of pesticide limits. |
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