| 方世翊,龙鼎新,袁建辉.改良QuEChERS的高效液相色谱-串联质谱法检测室内灰尘中5种拟除虫菊酯类农药残留.[J].中南医学科学杂志.,2024,(6):892-895. |
| 改良QuEChERS的高效液相色谱-串联质谱法检测室内灰尘中5种拟除虫菊酯类农药残留 |
| Detection of 5 pyrethroid pesticide residues in indoor dust by improved QuEChERS high performance liquid chromatography-tandem mass spectrometry method |
| 投稿时间：2024-03-24 修订日期：2024-10-28 |
| DOI：10.15972/j.cnki.43-1509/r.2024.06.004 |
| 中文关键词: 拟除虫菊酯 室内灰尘 高效液相色谱-串联质谱法 农药残留 改良QuEChERS法 |
| 英文关键词:pyrethroid indoor dust HLPC-MS/MS pesticide residue improved QuEChERS method |
| 基金项目:深圳市基础研究专项(JCYJ20210324131213037) 作者简介:方世翊,硕士研究生,研究方向为劳动卫生与环境卫生学,E-mail为13107498145@163.com。通信作者龙鼎新,博士,教授,博士研究生导师,研究方向为卫生毒理学,E-mail为dxlong99@163.com；通信作者袁建辉,博士,主任技师,博士研究生导师,研究方向为卫生毒理学,E-mail为jianhui_yuan@126.com。 |
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| 中文摘要: |
| 目的建立一种高效检测灰尘中拟除虫菊酯类农药残留的方法。 方法从使用过拟除虫菊酯类杀虫剂的居民家庭及办公场所收集灰尘样品,配制5种拟除虫菊酯(联苯菊酯、溴氰菊酯、氯菊酯、三氟氯氰菊酯、甲氰菊酯)混合标准液。使用ACQUITY HSS T3色谱柱分离,甲醇与5 mmol/L乙酸铵水溶液为流动相并优化梯度洗脱程序,电喷雾电离,正离子扫描,在多反应监测模式下分析。比较从灰尘样品中获取5种拟除虫菊酯的QuEChERS法、机械震荡法、超声萃取法的回收率。评估样品经QuEChERS法处理及上机后5种拟除虫菊酯的基质效应、线性度、检出限、回收率与相对标准偏差。 结果5种拟除虫菊酯在12 min内全部洗脱,分离良好；在5～100 μg/L范围内有良好的线性关系,相关系数均＞0.994；检出限为1.8~4.0 μg/kg；在20、60、100 μg/kg的加标范围内回收率为78.2%～106.2%,相对标准偏差均＜10%。成功建立了在灰尘样品中测定拟除虫菊酯残留量的改良QuEChERS的高效液相色谱-串联质谱法。 结论建立的改良QuEChERS的高效液相色谱-串联质谱法便捷有效,在保证准确率与精密度的同时,能够在短时间内精准检出灰尘样品中5种拟除虫菊酯农药。 |
| 英文摘要: |
| AimTo establish an efficient method for detecting pyrethroid pesticide residues in dust. MethodsDust samples from households and workplaces that have used pyrethroid insecticides were collected, and were prepared 5 mixed standard solutions of pyrethroids (bifenthrin, deltamethrin, cypermethrin, cyhalothrin, cypermethrin). Chromatographic column for separation by ACQUITY HSS T3, methanol and 5 mmol/L ammonium acetate aqueous solution as mobile phase and optimize gradient elution procedure, electrospray ionization, positive ion scanning, and analysis in multi reaction monitoring mode. The recovery rates of five pyrethroids obtained from dust samples were compared by using QuEChERS method, mechanical oscillation method, and ultrasonic extraction method. The matrix effect, linearity, detection limit, recovery rate, and relative standard deviation of the five pyrethroids after treatment with QuEChERS method and on the machine were evaluated. ResultsAll five pyrethroids were eluted within 12 min with good separation. The calibration curves showed good linearity in the range of 5－100 μg/L with the correlation coefficients ＞0.994. The limits of detection were 1.8－4.0 μg/kg. The recoveries were 78.2%－106.2% in the spiked ranges of 20,60, and 100 μg/kg, respectively, and the relative standard deviations ＜10%. An improved QuEChERS high performance liquid chromatography-tandem mass spectrometry method for determining pyrethroid residues in dust samples is successfully established. ConclusionThe high-performance liquid chromatography-tandem mass spectrometry method is convenient and effective, ensuring accuracy and precision while accurately detecting 5 types of pyrethroid pesticides in dust samples in a short period of time. |
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