基于HPLC-MS/MS的红枣中氯吡脲与赤霉酸同时检测方法的建立

Simultaneous Determination of Forchlorfenuron and Gibberellin Acid in Jujube Based on High Performance Liquid Chromatography-Mass-Mass Spectrometry

为建立红枣中氯吡脲(4-CPPU)和赤霉酸(GA3)两种植物生长调节剂残留的高效液相色谱-质谱方法 (HPLC-MS),用甲醇超声波提取法提取,经Sep-pakRVac 3cc(200 mg)C18固相萃取小柱净化,使用AgilentSBC18色谱柱(50 mm×2.1 mm,1.8μm)分离,在电喷雾离子源(ESI)多反应监测(MRM)离子扫描模式下做HPLCMS检测。试验结果表明:在建立的检测方法条件下,氯吡脲和赤霉酸均在10～100 ng/mL检测范围呈线性关系,相关系数均大于0.99;氯吡脲和赤霉酸的检出限均为7 ng/mL,定量限分别为22 ng/mL和25 ng/mL,平均回收率分别为88.5%和93.3%,平均相对标准偏差分别为3.7%和3.8%,达到检测要求。该方法可用于红枣中氯吡脲和赤霉酸的残留测定。

A qualitative and quantitative analysis method was established for determination of forchlorfenuron（4-CPPU） and gibberellin acid（GA3） in jujube（Ziziphus jujuba cv.Huizao and Junzao） using high performance liquid chromatography-mass-mass-spectrometry（HPLC-MS/MS）.The sample was extracted with methanol by ultrasonic extraction,and cleaned-up with Sep-pakRVac 3cc（200mg）C18solid phase extraction column.The separations were performed on AgilentSB-C18column（50 mm×2.1 mm,1.8 μm） and detected by electrospray ionization（ESI-） under multiple reaction monitoring（MRM） mode.The results showed that under conditions of the established detection method,gibberellin acid and forchlorfenuron represented a good linear relationships and the correlation coefficients greater than 0.99 were obtained at 10～100 ng/mL detection range.The limits of detection（LOD） both were 7 ng/mL while the limits of quantification were 22 ng/mL and 25 ng/mL for 4-CPPU and GA3,respectively.The recoveries were 88.5% and 93.3% with the relative standard deviations of 3.7% and 3.8% for 4-CPPU and GA3,respectively.The results indicate that the method is accurate and can be used for the determination of 4-CPPU and GA3residues in Jujube.