建立了基质固相分散萃取-高效液相色谱-串联质谱法(MSPD-HPLC-MS/MS)同时测定拟南芥中3种赤霉素GA1,GA3和GA4的分析方法.将拟南芥样品与C18填料混合研磨制成MSPD柱,并采用80％冷甲醇洗脱.采用反相C18色谱柱进行分离,以0.05％甲酸水溶液和乙腈为流动相进行梯度洗脱,采用电喷雾离子源负离子模式(ESI -)电离,多反应监测模式检测.对样品前处理条件、色谱分离条件和质谱检测条件进行了优化,结果表明,在最优条件下,3种赤霉素在10 ～ 300 ng/g范围内均呈良好线性关系,相关系数(r2)均大于0.98,检出限在1.1 ～4.1ng/g之间.在10 ～50 ng/g添加水平下,平均回收率范围为54.7％ ～102.6％,相对标准偏差(RSD,n=3)为3.2％～12.8％.该方法操作简单、灵敏度高、选择性好、回收率高,适合拟南芥中GA1、GA3、GA4含量的测定.%A method for the analysis of gibberellin A, (GA,), gibberellin A3 (GA3) and gibberel-lin A4 (GA4) in Arabidopsis thaliana by matrix solid-phase dispersion extraction (MSPD) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed. The solid sample of Arabidopsis thaliana was gently blended with C18 to obtain a homogeneous mixture. This mixture was transferred to an SPE cartridge filled with 0. 5 g C18 to form a MSPD column. GA,, GA3 and GA4 were eluted with cold 80% methanol aqueous solution. The target compounds were separated on a C18 column with a gradient elution of 0. 05% formic acid aqueous solution and acetonitrile as the mobile phase. The identification and quantification were carried out by using electrospray ionization in negative ion mode (ESI ~ ) with multiple reaction monitoring (MRM). The linear ranges for GA,, GA3 and GA4 were all from 10 to 300 ng/g with correlation coefficients greater than 0. 98. The limits of detection were in the range of 1. 1 - 4. 1 ng/g. The average recoveries and relative standard deviations were 54. 7% -102. 6% and 3. 2% - 12. 8% respectively in the spiked range of 10 - 50 ng/g. The method is simple, sensitive, efficient and accurate. It is suitable for the confirmation and quantitative determination of GA,, GA3 and GA4 in Arabidopsis thaliana.
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