| 李丹娜,王建山.QuEChERS-超高效液相色谱串联质谱法测定大米中30种农药残留[J].中国粮油学报,2024,39(4):165-170 |
| QuEChERS-超高效液相色谱串联质谱法测定大米中30种农药残留 |
| QuEChERS-Ultra-high-performance liquid chromatography-tandem mass spectrometry method for the determination of 30 pesticide residues in rice |
| 投稿时间：2023-04-18 修订日期：2023-08-06 |
| DOI： |
| 中文关键词: QuEChERS UPLC-MS/MS 大米 农药残留 |
| 英文关键词:QuEChERS UPLC-MS/MS rice pesticide residue |
| 基金项目:2019年陕西省创新能力支撑计划项目(2019PT-22) |
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| 中文摘要: |
| 采用QuEChERS前处理技术，结合超高效液相色谱串联质谱联用仪，建立大米中30种农药残留的测定方法。优化样品的提取溶剂、净化方式、液相色谱的分离条件和质谱参数等技术指标，采用优化后的条件，大米样品经1%乙酸乙腈提取，QuEChERS法净化后，用0.1%甲酸水（含2mmol/L甲酸铵）和甲醇为流动相，经Eclipse Plus C18 (2.1 mm×50 mm, 1.8 μm)分离, 采用电喷雾电离(electrospray ionization, ESI)和多离子检测模式(multiple reaction monitoring, MRM)进行检测, 基质外标法定量。30种农药的质量浓度在0.001~0.050 mg/L内与峰响应呈线性关系，线性相关系数均大于0.995，定量限（10S/N）在0.02~2.98 μg/kg，在3~30μg/kg添加浓度范围内, 平均回收率在70.3%~109.8%，相对标准偏差在1.1%~11.4%。该方法操作简单，方法稳健可行，可用于大米中农药残留的监测。 |
| 英文摘要: |
| The purpose of this study was to develop a method for the determination of 30 pesticide residues in rice using QuEChERS sample preparation technique and ultra-high-performance liquid chromatography-tandem mass spectrometry.The extraction solvent, purification method, chromatographic separation conditions, and mass spectrometry parameters were optimized. The optimized method involved extracting rice samples with 1% acetonitrile , followed by QuEChERS cleanup. Chromatographic separation was achieved using an Eclipse Plus C18 column (2.1 mm×50 mm, 1.8 μm) with a mobile phase of 0.1% formic acid water (containing 2 mmol/L ammonium formate) and methanol. Detection was performed using electrospray ionization (ESI) and multiple reaction monitoring (MRM) mode, and matrix-matched calibration was used for quantification.The calibration curves of the 30 pesticides showed good linearity over the concentration range of 0.001~0.050 mg/L, with correlation coefficients greater than 0.995. The limits of quantification (LOQs) were between 1 and 10 μg/kg, and the recoveries ranged from 70.3% to 109.8% with relative standard deviations (n=6) of 1.1-11.4% in the range of 3-30 μg/kg.The developed method was found to be simple, robust, and reliable, and is suitable for the monitoring of pesticide residues in rice. The proposed method may be used as a reference for pesticide residue detection in rice, and the results of this study may have important implications for food safety and environmental protection. |
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