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

Determination of paclobutrazol residue in citrus by QuEChERS-high performance liquid chromatography-tandem mass spectrometry

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

中文摘要:

      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。

英文摘要:

      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.