基质分散固相萃取-高效液相色谱-串联质谱法检测红薯中的植物生长调节剂  

Determination of the plant growth regulators in batatas by matrix solid-phase dispersive extraction and high performance liquid chromatography with tandem mass spectrometry

作　　者：张婧[1] 万慧慧[1] 张华[1] 

机构地区：[1]大连理工大学化工与环境生命学部化学分析测试中心,辽宁大连116024

出　　处：《色谱》2017年第9期963-969,共7页Chinese Journal of Chromatography

基　　金：国家自然科学基金项目(21505014);大连理工大学引进人才科研专题项目(DUT15RC(4)13)~~

摘　　要：建立了基质分散固相萃取-高效液相色谱-串联质谱测定红薯中氯吡脲、6-苄氨基嘌呤、增效胺以及多效唑含量的方法。样品经硅胶分散剂研磨分散、甲醇洗脱提取后,采用Thermo hypersil GOLD C18色谱柱(150 mm×2.1mm,5μm),以甲醇和0.1%(体积分数)甲酸-5 mmol/L甲酸铵为流动相进行梯度洗脱,在电喷雾离子源正离子或负离子模式下以选择反应监测(SRM)模式检测,外标法定量。氯吡脲、6-苄氨基嘌呤、增效胺和多效唑分别在10.8~216.0、10.8~216.0、12.5~250.0和10.2~204.0 ng/g范围内呈良好的线性关系,相关系数(r2)均大于0.96。以信噪比等于10确定4种植物生长调节剂的定量限,氯吡脲、6-苄氨基嘌呤、增效胺和多效唑的定量限分别为0.1、0.3、0.2和0.1 ng/g。4种植物生长调节剂在50、100及200 ng/g加标水平下的回收率为85.3%~116.0%,相对标准偏差为0.6%~22.7%。该方法操作简单、准确,适用于红薯中氯吡脲、6-苄氨基嘌呤、增效胺以及多效唑的定量检测分析。An analytical method based on matrix solid-phase dispersive （MSPD） extraction and high performance liquid chromatography-tandem mass spectrometry （ HPLC-MS/MS） was established for the determination of forchlorfenuron, 6-benzylaminopurine （6-BA）, N- （2-ethyl- hexyl） -5-norbornene-2,3-dicarboximide （MGK 264） and paclobutrazol in batatas. The samples were dispersed with silica by grinding,and then extracted with methanol. The determination was carried out on a Thermo hypersil GOLD C18 column （150 mmx2. 1 mm,5 μm） in gradient elution with mobile phases of methanol and ammonium formate （5 mmol/L ,containing 0. 1%（v/v ） formic acid） and detected with tandem mass spectrometry using selected reaction moni-toring （SRM） mode. The quantification was performed using external standard calibration,and the calibration curves were performed in the ranges of 10. 8-216.0 ng/g （ forchlorfenuron ）, 10.8-216.0 ng/g （6-BA）,12.5-250.0 ng/g （MGK 264）,10.2-204.0 ng/g （paclobutrazol） with the correlation coefficients larger than 0. 96. The limits of quantification （LOQs） were 0. 1 -0.3 ng/g. The spiked recoveries at the levels of 50, 100 and 200 ng/g of these four plant growth regulators were in the range of 85. 3% -116. 0%,and the relative standard deviations were 0.6%-22.7%. This method has advantages of simple operation and good accuracy, and can be used for the quantitative determination of forchlorfenuron, 6-BA,MGK 264 and paclobutrazol in batatas.

关 键 词：基质分散固相萃取 高效液相色谱-串联质谱 氯吡脲 6-苄氨基嘌呤 增效胺 多效唑 红薯 

分 类 号：O658[理学—分析化学]