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

作　　者：周勇[1] 刘佳[1] 朱航[1] 马海昊[1] 刘哲铭 贾楠 霍晓宜 周小毛[1] ZHOU Yong;LIU Jia;ZHU Hang;MA Hai-Hao;LIU Zhe-Ming;JIA Nan;HUO Xiao-Yi;ZHOU Xiao-Mao(Institute of Biotechnology,Hunan Academy of Agricultural Sciences,Hunan Academy of Agricultural Science,Changsha 410125,China)

机构地区：[1]湖南省农业科学院湖南省农业生物技术研究所,长沙410125

出　　处：《食品安全质量检测学报》2020年第15期4995-5000,共6页Journal of Food Safety and Quality

基　　金：国家重点研发计划项目(2017YFD0200308)。

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, 1.9μm)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.

关 键 词：多效唑 QUECHERS 高效液相色谱-串联质谱法 柑橘 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]