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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。
In order to establish a HPLC-MS method for the determination of phytoflue residues (4-CPPU) and gibberellic acid (GA3) in jujube jujube and extract them by ultrasonic extraction with methanol, The pakRVac 3cc (200 mg) C18 solid phase extraction cartridges were purified on an AgilentSBC18 column (50 mm × 2.1 mm, 1.8 μm) for HPLCMS in Electrospray Ionization Source (ESI) Multiple Reaction Monitoring (MRM) Detection. The results showed that the calibration curves of clopidofur and gibberellic acid were linear in the range of 10-100 ng / mL with the correlation coefficients greater than 0.99. The detection limits of clopidamide and gibberellic acid The average recoveries were 88.5% and 93.3%, respectively. The average relative standard deviations were 3.7% and 3.8%, respectively. The detection limits were met. The method can be used for the determination of clopidogrel and gibberellic acid residues in jujube.