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.
出处
《色谱》
CAS
CSCD
北大核心
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)
关键词
QUECHERS
高效液相色谱-串联质谱法
植物生长调节剂
水果
QuEChERS
high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)
plant growth regulators
fruits