QuEChERS-高效液相色谱-串联质谱法同时测定水果中21种植物生长调节剂的残留量  

Determination of 21 plant growth regulator residues in fruits by QuEChERS-highperformance liquid chromatography-tandem mass spectrometry

作　　者：黄何何[1,2] 张缙[1] 徐敦明[1] 周昱[1] 罗佳[2] 吕美玲[3] 陈树宾[4] 王连珠[1] 

机构地区：[1]厦门出入境检验检疫局,福建厦门361026 [2]福建农林大学,福建福州350002 [3]安捷伦科技(中国)有限公司,北京100102 [4]宁波出入境检验检疫局,浙江宁波315000

出　　处：《色谱》2014年第7期707-716,共10页Chinese Journal of Chromatography

基　　金：福建省自然科学基金项目(2013J01031);浙江省公益性技术应用研究计划项目(2012C37074)

摘　　要：建立了高效液相色谱-串联质谱法（HPLC-MS/MS）同时测定水果中21种植物生长调节剂残留量的方法。样品经QuEChERS法进行预处理,选用含1%（v/v）乙酸的乙腈溶液提取,无水硫酸镁和十八烷基硅烷（C18）粉末净化,以C18色谱柱分离待测物,采用鞘流电喷雾离子化,正负离子分段扫描和多反应监测模式（MRM）检测,基质匹配标准溶液外标法定量。矮壮素、助壮素、氯化胆碱、环丙酸酰胺、氯吡脲、噻苯隆、抗倒胺、多效唑、烯效唑和抑芽唑在0.10-500μg/L,丁酰肼和6-苄氨基嘌呤在1.0-500μg/L,2,3,5-三碘苯甲酸、2,4-D、调果酸、对氯苯氧乙酸（4-CPA）和抗倒酯在2.0-1 000μg/L,赤霉素（GA3）、脱落酸（ABA）、1-萘乙酸（NAA）和吲哚-3-乙酸（IAA）在10-1 000μg/L的范围内线性关系良好,相关系数均大于0.990。21种植物生长调节剂的方法检出限为0.020-6.0μg/kg,方法定量限为0.10-15.0μg/kg,样品添加回收试验的平均回收率为73.0%-111.0%,相对标准偏差为3.0%-17.2%（n=6）。该方法快速简便,定量准确,可满足多种水果中21种植物生长调节剂的残留检测要求。A method for the simultaneous detection of 21 plant growth regulators in fruits by QuEChERS-high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）was developed.The samples were initially extracted with acetonitrile containing 1%（v/v）acetic acid,followed by clean-up using the powder of magnesium sulfate and C18.The resulting samples were separated on a C18 column,and detected under positive and negative multiple reactions monitoring（MRM）mode through polarity switching between time segments.The matrix-matched external standard calibration curves were used for quantitative analysis.The linearities of chlormequat chloride,mepiquat chloride,choline chloride,cyclanilide,forchlorfenuron,thidiazuron,inabenfide,paclobutrazol,uniconazole and triapenthenol were in the concentration range of 0.1-500μg/L,daminozide and 6-benzylaminopurine in the concentration range of 1.0-500μg/L,2,3,5-triiodobenzoic acid,2,4-D,cloprop,4-chlorophenoxyacetic acid（4-CPA）and trinexapac-ethyl in the concentration range of 2.0-1 000μg/L,abscisic acid（ABA）,gibberellic acid（GA3）,1-naph-thaleneacetic acid（NAA）and indol-3-ylacetic acid（IAA）in the concentration range of 10-1 000μg/L,with the correlation coefficients higher than0.990.The limits of detection and the limits of quantification of the method were 0.020-6.0μg/kg and 0.10-15.0μg/kg,respectively.For all the samples,the average spiked recoveries ranged from73.0%to 111.0%,and the relative standard deviations（RSDs,n=6）were in the range of 3.0%-17.2%.The method is quick,easy,effective,sensitive and accurate,and can meet the requirements for the determination of the 21 plant growth regulator residues in fruits.

关 键 词：QUECHERS 高效液相色谱-串联质谱法 植物生长调节剂 水果 

分 类 号：O658[理学—分析化学]