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中国精品科技期刊2020
彭红霞,刘娅,杨丽,等. QuEChERS-超高效液相色谱法测定谷物及油籽中氰氟草酯和氰氟草酸残留量[J]. 食品工业科技,2022,43(11):310−317. doi: 10.13386/j.issn1002-0306.2021090139.
引用本文: 彭红霞,刘娅,杨丽,等. QuEChERS-超高效液相色谱法测定谷物及油籽中氰氟草酯和氰氟草酸残留量[J]. 食品工业科技,2022,43(11):310−317. doi: 10.13386/j.issn1002-0306.2021090139.
PENG Hongxia, LIU Ya, YANG Li, et al. Determination of Cyhalofop-butyl and Cyhalofop-acid Residues in Cereals and Oilseeds by QuEChERS-UPLC[J]. Science and Technology of Food Industry, 2022, 43(11): 310−317. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021090139.
Citation: PENG Hongxia, LIU Ya, YANG Li, et al. Determination of Cyhalofop-butyl and Cyhalofop-acid Residues in Cereals and Oilseeds by QuEChERS-UPLC[J]. Science and Technology of Food Industry, 2022, 43(11): 310−317. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021090139.

QuEChERS-超高效液相色谱法测定谷物及油籽中氰氟草酯和氰氟草酸残留量

Determination of Cyhalofop-butyl and Cyhalofop-acid Residues in Cereals and Oilseeds by QuEChERS-UPLC

  • 摘要: 目的:建立了一种能同时检测谷物和油籽中氰氟草酯和氰氟草酸残留量的QuEChERS-超高效液相色谱法。方法:称取样品2.0 g和5.0 g,用0.1%甲酸水-乙腈(1:1,V/V)提取,经N-丙基乙二胺(PSA)、C18、氯化钠、无水硫酸镁等净化后,过0.22 μm滤膜,以0.1% 磷酸水溶液-甲醇-乙腈为流动相进行梯度洗脱,使用ACQUITY UPLC BEH C18(50 mm× 2.1 mm, 1.7 μm)色谱柱分离,UPLC分析检测,外标法定量。结果:在0.002~5 μg/mL范围内,氰氟草酯和氰氟草酸的质量浓度与峰面积呈良好的线性关系,谷物和油籽中的定量限浓度分别为0.01 mg/kg和0.02 mg/kg。谷物中氰氟草酯和氰氟草酸加标回收率分别为89.23%~101.12%和87.98%~100.02%,油籽中分别为85.12%~92.34%和82.63%~89.55%,相对标准偏差均为1.1%~3.3%。结论:该方法前处理过程简单,检测过程准确、高效,灵敏度和准确度达到了农残检测的要求,适用于谷物和油籽中氰氟草酯和氰氟草酸的残留检测。

     

    Abstract: Objective: The method of QuEChERS-UPLC was established for the simultaneous determination of cyhalofop-butyl and cyhalofop-acid residues in cereals and oilseeds. Methods: The accurately weighed 2.0 g and 5.0 g sample was extracted with 0.1% formic acid water-acetonitrile (1:1, V/V) as extractant, and then purified with dispersive solid phase extraction adsorbents, such as N-propyl ethylenediamine (PSA), C18, sodium chloride, anhydrous magnesium sulfate, etc. After the purified solution was filtered through a 0.22 μm filter membrane, it was eluted with 0.1% phosphoric acid aqueous solution-methanol-acetonitrile as the mobile phase for gradient elution, separated by ACQUITY UPLC BEH C18 (50 mm × 2.1 mm, 1.7 μm) chromatographic column, analyzed and detected by UPLC, and quantified by external standard method. Results: In the range of 0.002~5 μg/mL, the mass concentration of cyhalofop-butyl and cyhalofop-acid showed a good linear relationship with the peak area, and the limits of quantification in grains and oilseeds were 0.01 mg/kg and 0.02 mg/kg, respectively. The recoveries of cyhalofop-butyl and cyhalofop-acid in cereals were 89.23%~101.12% and 87.98%~100.02%. Those in oilseeds were 85.12%~92.34% and 82.63%~89.55% respectively. The relative standard deviation was 1.1%~3.3%. Conclusion: The method used in this experiment has a simple pretreatment process, accurate and efficient detection process, and its sensitivity and accuracy meet the requirements of pesticide residue detection. It is suitable for the detection of cyhalofop-butyl and cyhalofop-acid residues in grains and oilseeds.

     

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