高效液相色谱-串联质谱法测定水果中多种 天然植物生长调剂的残留量
目的 采用高效液相色谱-串联质谱法建立了同时测定水果中赤霉素GA3、吲哚-3-乙酸和1-萘乙酸3种天然植物生长调剂残留的检测方法。方法 样品经QuEChERS法进行预处理, 以1%乙酸乙腈提取, 无水硫酸镁和C18粉末净化。选用水-乙腈为流动相, C18色谱柱分离, 采用Agilent AJS ESI源、负离子扫描和多反应检测模式(MRM)进行质谱检测, 基质匹配标准溶液外标法定量。结果 3种天然植物生长调剂在0.005?1.000 mg/L浓度范围内线性关系良好, 赤霉素GA3的方法定量限(S/N=10)分别为0.010 mg/kg, 吲哚-3-乙酸和1-萘乙酸均为0.005 mg/kg。对空白水果样品进行0.020、0.050、0.100 mg/kg 3个添加水平的回收实验, 赤霉素GA3、吲哚-3-乙酸和1-萘乙酸的回收率分别为75.4%~109.8%、79.1%~109.3%和79.6%~112.9%, 相对标准偏差(n=6)分别为3.5%~17.4%、6.5%~15.8%和4.8%~13.9%。结论 该方法快速简便, 定量准确, 可满足水果中3种农药的残留检测要求。
Objective To develop a method for the simultaneous detection of GA3, IAA and NAA in fruits by QuEChERS-HPLC-ESI-MS/MS. Methods The samples were extracted with acetonitrile with 1% acetic acid, purified using powder of magnesium sulfate and C18. Three pesticides were separated on a C18 column with the mobile phases of water and acetonitrile and finally detected with negative electrospray ionization in MRM mode. The matrix-matched external standard calibration curves were used for quantitative analysis. Results The linearities of GA3, IAA and NAA were in the concentration ranges of 0.005?1.000 mg/L, with the correlation coefficients higher than 0.9990 for the 3 pesticides. The limit of quantification (LOQ) were 0.010 mg/kg for GA3, 0.005 mg/kg for IAA and NAA. For all the samples, the mean spiked recoveries of GA3, IAA and NAA ranged from 75.4%?109.8%, 79.1%~109.3% and 79.6%~112.9%, respectively, and the relative standard deviations (RSD, n=6) were in the range of 3.5%~17.4%, 6.5%~15.8% and 4.8%~13.9%, respectively. Conclusion The method is quick, easy, effective, sensitive and accurate, and it can meet the requirements for the determination of GA3, IAA and NAA pesticide residues in fruits.
标题：高效液相色谱-串联质谱法测定水果中多种 天然植物生长调剂的残留量
英文标题：Determination of several natural plant growth regulators in fruits by high performance liquid chromatography-tandem mass spectrometry
作者：
黄何何 1.福建农林大学植物保护学院;2.厦门出入境检验检疫局检验检疫技术中心
徐敦明 厦门出入境检验检疫局检验检疫技术中心
周昱 厦门出入境检验检疫局检验检疫技术中心
罗佳 福建农林大学植物保护学院
吕美玲 安捷伦科技(中国)有限公司
陈树宾 宁波出入境检验检疫局检验检疫技术中心
王连珠 厦门出入境检验检疫局检验检疫技术中心
中文关键词:高效液相色谱-串联质谱,天然植物生长调剂,水果,
英文关键词:high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS),natural plant growth regulator,fruits,
发表日期：2014-01-17
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