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目的建立水果中4-氯苯氧乙酸、氯吡脲和2,4-二氯苯氧乙酸3种植物激素残留量的超高效液相色谱测定方法。方法样品经乙腈匀浆提取,经氨基固相萃取小柱净化后,采用Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm),以乙腈-0.1%磷酸为流动相,梯度洗脱,流速:0.2 ml/min,柱温:35℃,检测波长为230 nm,外标法峰面积定量。结果 4-氯苯氧乙酸、氯吡脲、2,4-二氯苯氧乙酸在1μg/ml~100μg/ml时与峰面积呈良好的线性关系,相关系数为0.999 5~0.999 8,平均回收率为75%~97%,相对标准偏差为0.5%~1.1%,检出限为0.10 mg/kg~0.20 mg/kg。结论该法简单快速灵敏度高,适用于日常水果的检测。
OBJECTIVE To establish a method for the determination of 3 hormones residues in fruits of 4-chlorophenoxyacetic acid, clopidogrel and 2,4-dichlorophenoxyacetic acid by ultra performance liquid chromatography. Methods The samples were extracted with acetonitrile and purified by Amino Solid Phase Extraction (SPE) cartridges. The mobile phases were eluted with a Waters ACQUITY UPLC BEH C18 column (2.1 mm × 100 mm, 1.7 μm) with acetonitrile-0.1% phosphoric acid , The flow rate was 0.2 ml / min, the column temperature was 35 ℃, the detection wavelength was 230 nm, and the external standard peak area was quantified. Results 4-Chlorphenoxyacetic acid, clopidamide and 2,4-dichlorophenoxyacetic acid showed a good linear relationship with the peak area at the concentration of 1μg / ml ~ 100μg / ml, the correlation coefficient was 0.999 5 ~ 0.999 8, the average recovery The relative standard deviations ranged from 75% to 97% with relative standard deviations from 0.5% to 1.1% with a detection limit of 0.10 mg / kg to 0.20 mg / kg. Conclusion The method is simple and fast and sensitive, suitable for the detection of daily fruits.