QuEChERS结合高效液相色谱串联质谱法测定柑橘中多效唑残留量
目的 建立高效液相色谱串联质谱法(high performance liquid chromatography?tandem mass spectrometry, HPLC?MS/MS)测定柑橘中多效唑残留量的分析方法。方法 样品采用QuEChERS (quick, easy, cheap, effective, rugged, safety)方法进行前处理, 用乙腈提取, N-丙基乙二胺(N-Propylethylenediamine, PSA)和无水硫酸镁净化, 并采用HPLC-MS/MS检测。采用Hypersil GOLD C18色谱柱(100 mm×2.1 mm, 1.9 μm)进行分离, 0.1%甲酸水溶液-甲醇溶液作为流动相进行梯度洗脱, 洗脱流速为0.3 mL/min, 柱温为35 ℃。结果 多效唑在0.0005~1.0 mg/L浓度范围内的相关系数r2=0.9981, 呈现良好的线性关系。在0.002、0.2和2 mg/kg添加水平下, 多效唑在柑橘全果、果肉和果皮中的平均添加回收率范围为80.9%~102.7%, 相对标准偏差范围为4.1%~13.1%, 方法的定量限均为0.002 mg/kg。结论 该方法操作简便、准确度高、回收率及精密度好, 适用于柑橘中多效唑残留量的检测。
Objective To establish a method for the determination of paclobutrazol residue in citrus by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The samples were pretreated by QuEChERS (quick, easy, cheap, effective, rugged, safe), extracted by acetonitrile, purified by N-propylethylenediamine (PSA) and anhydrous magnesium sulfate, and detected by HPLC-MS/MS. A Hypersil GOLD C18 column (100 mm×2.1 mm, 1.9 m) was used for separation, and 0.1% formic acid aqueous solution-methanol solution was used as mobile phase for gradient elution, the elution flow rate was 0.3 mL/min, and the column temperature was 35 ℃. Results The correlation coefficient r2 of paclobutrazol in the range of 0.0005-1.0 mg/L was 0.9981, showing a good linear relationship. The average recoveries and relative standard deviations of paclobutrazol in citrus fruit, pulp and pericarp were 80.9%–102.7%, 4.1%–13.1% and 0.002 mg/kg respectively at 0.002, 0.2 and 2 mg/kg levels. Conclusion This method is simple to operate, high in accuracy, good in recovery rate and precision, and is suitable for the detection of paclobutrazol residues in citrus.
标题：QuEChERS结合高效液相色谱串联质谱法测定柑橘中多效唑残留量
英文标题：Determination of paclobutrazol residue in citrus by QuEChERS-high performance liquid chromatography-tandem mass spectrometry
作者：
周勇 湖南省农业科学院湖南省农业生物技术研究所
刘佳 湖南省农业科学院湖南省农业生物技术研究所
朱航 湖南省农业科学院湖南省农业生物技术研究所
马海昊 湖南省农业科学院湖南省农业生物技术研究所
刘哲铭 湖南省农业科学院湖南省农业生物技术研究所
贾楠 湖南省农业科学院湖南省农业生物技术研究所
霍晓宜 湖南省农业科学院湖南省农业生物技术研究所
周小毛 湖南省农业科学院湖南省农业生物技术研究所
中文关键词:多效唑,QuEChERS,高效液相色谱-串联质谱法,柑橘,
英文关键词:paclobutrazol,QuEChERS,high performance liquid chromatography‒tandem mass spectrometry,citrus,
发表日期：2020-04-23
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