| QuEChERS-高效液相色谱-串联质谱法检测吡噻菌胺、肟菌酯及代谢物在番茄中的残留及长期膳食风险评估 |
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| 引用本文： | 李若同,胡继业. QuEChERS-高效液相色谱-串联质谱法检测吡噻菌胺、肟菌酯及代谢物在番茄中的残留及长期膳食风险评估[J]. 农药学学报, 2022, 24(3): 572-580. DOI: 10.16801/j.issn.1008-7303.2021.0183 |
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| 作者姓名： | 李若同 胡继业 |
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| 作者单位： | 1.北京科技大学 化学与生物工程学院,北京 100083 |
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| 摘 要： | 建立了吡噻菌胺及其主要代谢物1-甲基-3- (三氟甲基)-1H-吡唑-4-甲酰胺 (PAM)和肟菌酯及其代谢物肟菌酸在番茄中残留的分析方法。样品经乙酸-乙腈提取,无水硫酸镁、N-丙基乙二胺 (PSA)和石墨化碳黑 (GCB)净化,高效液相色谱-串联质谱 (HPLC-MS/MS)检测。结果表明:吡噻菌胺、PAM、肟菌酯和肟菌酸在0.025~2 mg/L范围内的线性关系良好,R2≥0.999 2。在不同添加水平下,4种化合物在番茄中的平均回收率在88%~97%之间,相对标准偏差 (RSD)小于3.9%,定量限 (LOQ)均为0.05 mg/kg。按照《农作物中农药残留试验准则》在全国12个地区开展规范残留试验,30%吡噻菌胺 ? 肟菌酯悬浮剂以推荐剂量有效成分270 g/hm2,于番茄灰霉病发生初期喷雾施药2次,施药间隔7 d (推荐的安全间隔期为5 d)。在分别于末次施药后5和7 d采集的番茄样品中,吡噻菌胺的残留量均低于0.26 mg/kg,肟菌酯的均低于0.33 mg/kg,均未超出中国制定的吡噻菌胺和肟菌酯在番茄中的最大残留限量 (MRL)值。根据田间残留试验结果、膳食结构和毒理学数据进行了长期膳食风险评估。结果表明:普通人群吡噻菌胺和肟菌酯国家估算每日摄入量 (NEDI)分别为0.1382和0.2645 mg,膳食风险商 (RQ)均小于100%,说明在推荐的良好农业规范 (GAP)条件下施用30%吡噻菌胺 ? 肟菌酯悬浮剂不会对人体健康产生不可接受的风险。
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| 关 键 词： | QuEChERS 高效液相色谱-串联质谱 吡噻菌胺 肟菌酯 代谢物 番茄 残留 膳食风险评估 |
| 收稿时间： | 2021-09-10 |
Residue and chronic dietary risk assessment of penthiopyrad,trifloxystrobin and their metabolites in tomato by QuEChERS-high performance liquid chromatography-tandem mass spectrometry |
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| Affiliation: | 1.School of Chemistry and Biological Engineering, University of Science and Technology Beijing, Beijing 100083, China |
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| Abstract: | A method was established for the simultaneous determination of penthiopyrad, its main metabolite 1-methyl-3-trifluoromethyl-1H-pyrazole-4-carboxamide (PAM), trifloxystrobin and its metabolite trifloxystrobin acid in tomato. The samples were extracted with acetic acid and acetonitrile, cleaned-up with anhydrous MgSO4, primary secondary amine (PSA) and GCB, and detected by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The linearities of penthiopyrad, PAM, trifloxystrobin and trifloxystrobin acid ranged from 0.025 to 2 mg/L, with R2≥ 0.9992. The average recoveries of the four compounds in tomato at different spiked levels were 88%-97%, with the relative standard deviations (RSD) less than 3.9%. The limits of quantification (LOQs) of the analytes were all 0.05 mg/kg. The supervised residue trials were carried out in 12 farm regions in China according to Guideline for the Testing of Pesticide Residues in Crops. The 30% suspension concentrate of penthiopyrad and trifloxystrobin was sprayed twice with an interval of 7 days at the recommended dosage of 270 g a.i./hm2 at the early stage of Botrytis cinerea in tomato, and the recommended pre-harvest interval was 5 days. On the 5th and 7th day after the last application, the residues of penthiopyrad in tomato samples were below 0.26 mg/kg, and the residues of trifloxystrobin were below 0.33 mg/kg, which were lower than the corresponding MRLs set in China. The dietary risk assessment was carried out according to the results of residue field trials, dietary structure and toxicological data. The results showed that the national estimated daily intake (NEDI) of penthiopyrad and trifloxystrobin were 0.1382 mg and 0.2645 mg, respectively. The dietary risk quotient (RQ) of penthiopyrad and trifloxystrobin in tomato were less than 100%, which indicated that the application of the 30% suspension concentrate of penthiopyrad and trifloxystrobin under recommended Good Agricultural Practice (GAP) conditions would not pose an unacceptable risk to human health. |
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