固相萃取/超高效液相色谱-串联质谱测定水果中5种植物生长调节剂残留量  

Determination of 5 Plant Growth Regulator Residues in Fruits by Solid Phase Extraction and Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：仲伶俐[1] 胡莉[1] 郭灵安[1] 雷绍荣[1] 毛建霏[1] 李曦[1] 欧阳华学[1] 

机构地区：[1]四川省农业科学院分析测试中心,四川成都610066

出　　处：《分析测试学报》2016年第4期466-470,共5页Journal of Instrumental Analysis

基　　金：四川省财政基因工程专项资金项目(2012QNJJ-026);四川省农业科学院新兴学科(2013XXXK-023)

摘　　要：建立了固相萃取/超高效液相色谱-串联质谱（UPLC-MS/MS）同时测定水果中6-苄基腺嘌呤（6-BA）、噻苯隆、氯吡脲、多效唑和烯效唑5种植物生长调节剂残留量的分析方法。水果样品经乙腈提取,NH2固相萃取小柱进行富集、净化,以二氯甲烷-甲醇（92∶8）为洗脱溶液,浓缩定容后,用Waters ACQUITY UPLC BEH C18（50 mm×2.1 mm,1.7μm）色谱柱分离,流速0.3 m L/min,以水-甲醇为流动相梯度洗脱,于UPLC-MS/MS仪多反应监测（MRM）模式测定,基质匹配标准溶液外标法定量。结果表明,5种植物生长调节剂在5-500 ng/m L浓度范围内呈良好的线性关系,相关系数（r^2）为0.996 1-0.999 6。在0.004,0.02,0.1 mg/kg加标水平下,方法的回收率为75.6%-110.5%,相对标准偏差（RSD）为1.2%-12.8%,方法检出限（LOD,S/N≥3）为0.001-0.002 mg/kg,定量下限（LOQ,S/N≥10）为0.003-0.006 mg/kg。该方法操作简便、灵敏度高、准确可靠,适用于水果中5种植物生长调节剂残留量的同时测定。A method for the simultaneous determination of 5 plant growth regulator residues,including 6-benzyl adenine（6-BA）,thidiazuron,forchlorfenuron,paclobutrazol and uniconazole in fruits was developed by using ultra high performance liquid chromatography-tandem mass spectrometry（UPLC-MS /MS） with solid phase extraction（SPE）.Samples were extracted with acetonitrile,then the extracts were concentrated and cleaned up on a NH2 solid phase extraction cartridge with dichloromethane-methanol（92 ∶ 8） as elution solution.Sample preparation was accomplished after concentrated and redissoved.The UPLC-MS / MS method was performed with Waters ACQUITY UPLC BEH C18（50 mm × 2.1 mm,1.7 μm） column using water-methanol as mobile phase by gradient elution,at a flow rate of 0.3 m L / min.The target compounds were determined by UPLC-MS / MS under multi reaction monitoring（MRM） mode,and then quantitatively analyzed by external standard method using the matrix-matched standard solution.The results showed that there were good linearities for 5 plant growth regulators between peak areas and concentrations in the range of 5-500 ng / m L under the optimal conditions,with correlation coefficients（r^2） of 0.996 1-0.999 6.The spiked recoveries of 5 plant growth regulators in fruits at three spiked levels of 0.004,0.02,0.1 mg / kg ranged from 75.6% to 110.5% with relative standard deviations（RSDs） of 1.2%-12.8%.The limits of detection of this method（LOD） were in the range of 0.001-0.002 mg / kg,and the limits of quantitation（LOQ） were 0.003-0.006 mg / kg.The established method was simple,sensitive,accurate and reliable,and could meet the requirements of multi pesticide residues analysis in fruits.

关 键 词：固相萃取 超高效液相色谱-串联质谱 水果 植物生长调节剂 

分 类 号：O657.63[理学—分析化学] TQ314.254[理学—化学]