超高效液相色谱串联质谱法测定果蔬中13种植物生长调节剂残留量  

Determination of 13 plant growth regulator residues in fruits and vegetables using ultra performance liquid chromatography tandem mass spectrometry

作　　者：林海丹[1] 谢守新[1] 王岚[1] 徐娟[1] 吴思彦 邹志飞[1] 

机构地区：[1]广东出入境检验检疫局检验检疫技术中心,广东广州510623 [2]广东药学院食品科学与工程系,广东广州510006

出　　处：《广东农业科学》2015年第9期82-87,共6页Guangdong Agricultural Sciences

基　　金：广东省科技计划项目(2011B010500015)

摘　　要：建立了超高效液相色谱串联质谱法同时测定果蔬13种植物生长调节剂残留量的方法.样品经甲醇水提取,用Shim-pack XR C18色谱柱（75 mm×2.0 mm,1.6μm）,以乙腈-0.1％乙酸溶液作为流动相梯度洗脱,采用电喷雾离子化,正、负离子扫描,多反应选择离子监测,基质匹配外标法峰面积定量.矮壮素、多效唑、烯效唑、噻苯隆、赤霉素、2-奈乙酸、氯吡脲、2,4-D、调果酸、4-氯苯氧乙酸、2,4,5-三氯苯氧乙酸、6-BA和氯苯胺灵在质量浓度1～20 μg/L范围内线性良好,相关系数r均大于0.99,样品在10、20、50 μg/kg等3个添加水平的平均回收率为81.2％～106％,变异系数为2.13％～11.8％ （n=6）,方法的定量限为0.022～16 μg/kg.该方法简便、特异性好,适用于果蔬中13种植物生长调节剂的检测.To develop a ultra performance liquid chromatography tandem mass spectrometry （UPLC-MS/ MS） method for the determination of 13 plant growth regulator residues in fruits and vegetables. The sample was extracted with methanol-H20 and the chromatographic separation was performed on the Shim-pack XR Cl8 column （75 mm×2.0 ram, 1.6μm） , using acetonitrile-0.1% acetic acid as the mobile phase by gradient elution. The method applied electrospray ionization in positive and negative multiple reaction monitoring mode and quantified with peak area with matrix-matched external standard method. A good linearity of Chlormequat chloride, Paclobutrazol, Uniconazole, thidiazuron, gibberellic acid 2-naphthaleneaeetic acid, Forchlorfenuron, 2, 4-D, Cloprop, 4-Chloroph-enoxyacetic acid, 2, 4, 5-Trichlorophenoxyacetic acid, 6-Benzylaminopurine and isopropyl N-（3-chlorophenyl） earbamate were in the concentration range of 1.0-20 μg/L with a correlation coefficient above 0.99. The average recoveries from three different were with the range of 81.2% to 106% at spiked levels of 10, 20, 50μg/kg, and the relative standard deviations were between 2.13% to 11.8% （n=6）. The limit of quantification was in the range of 0.022-16 μg/kg. This method is simple, selectivity and suitable for determination of 13 residues in fruits and vegetables.

关 键 词：高效液相色谱串联质谱 果蔬 植物生长调节剂 

分 类 号：O657.63[理学—分析化学]