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目的建立豆芽中2,4-二氯苯氧乙酸、4-氯苯氧乙酸、噻苯隆和6-苄氨基腺嘌呤的固相萃取-超快速液相色谱-串联质谱分析方法。方法豆芽经0.1%乙酸-乙腈溶液超声提取5 min,加入脱水试剂(6 g无水硫酸镁和1.5 g乙酸钠)涡旋,离心,上清液经Waters Oasis PRi ME固相萃取小柱净化,以乙腈和5 mmol/L乙酸铵-0.1%(V/V)氨水的混合溶液为流动相,采用梯度洗脱方式,在Acquity UPLC BEH C18柱(100 mm×2.1 mm,1.7μm)上进行分离,以电喷雾离子源(ESI)多反应监测(MRM)模式下检测,外标法定量。结果 4种植物生长调节剂的浓度为0.50μg/kg~100.0μg/kg时,呈现良好的线性关系,相关系数(r)均≥0.999 5,方法的定量限为0.07μg/kg~0.43μg/kg,加标回收率为88.5%~98.2%,相对标准偏差(RSD)为1.0%~8.2%。结论本方法可用于豆芽中2,4-二氯苯氧乙酸、4-氯苯氧乙酸、噻苯隆和6-苄氨基腺嘌呤等植物生长调节剂残留的快速筛查与分析。
Objective To establish a method for the determination of 2,4-dichlorophenoxyacetic acid, 4-chlorophenoxyacetic acid, thidiazuron and 6-benzyladenine in bean sprouts by ultra performance liquid chromatography-tandem mass spectrometry. Methods The sprouts were ultrasonically extracted with 0.1% acetic acid-acetonitrile for 5 min. The sprouts were spun by adding dehydration reagent (6 g anhydrous magnesium sulfate and 1.5 g sodium acetate), and the supernatant was purified by Waters Oasis PRi ME SPE cartridge. A gradient elution was performed on a Acquity UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 μm) using a mixture of acetonitrile and 5 mmol / L ammonium acetate-0.1% (V / V) , Electrospray ionization (ESI) multi-reaction monitoring (MRM) mode of detection, external standard quantitative. Results The results showed that there was a good linear relationship between the concentration of four plant growth regulators and 0.50μg / kg ~ 100.0μg / kg, the correlation coefficient (r) ≥0.9995. The limit of quantification was 0.07μg / kg ~ 0.43μg / kg, the spiked recoveries ranged from 88.5% to 98.2%, and the relative standard deviations (RSDs) ranged from 1.0% to 8.2%. Conclusion The method can be applied to the rapid screening and analysis of the residues of plant growth regulators such as 2,4-dichlorophenoxyacetic acid, 4-chlorophenoxyacetic acid, thidiazuron and 6-benzyladenine in bean sprout.