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目的建立基于自制混合型固相萃取柱净化样品-高效液相色谱同时测定豆芽中6-苄基腺嘌呤、异戊烯基腺嘌呤、赤霉素、4-氟苯氧乙酸、4-氯苯氧乙酸的方法。方法样品经20 ml乙腈提取,盐析离心,通过自制固相萃取柱净化,经Spursil C18-EP色谱柱分离,乙腈和0.5%磷酸为流动相,紫外检测器检测,检测波长为209 nm,外标法定量。结果 5种植物生长调节剂在0.5μg/ml~50μg/ml,线性良好,相关系数均>0.999;添加高、中、低3个浓度(1 mg/kg、10 mg/kg、40 mg/kg)作为加标,平均加标回收率为82.1%~110.2%;相对标准偏差(RSD)均<6.5%。检出限(S/N=3)为0.04 mg/kg~0.10 mg/kg,定量限(S/N=10)为0.06 mg/kg~0.30 mg/kg。结论采用自制混合固相萃取柱,样品处理简便、快捷。高效液相色谱法同时检测5种组分,可以保证准确度、灵敏度、精密度。降低时间、人员、环境成本,对于没有液相色谱质谱联用的基层单位,在豆芽检测中,具有一定的推广意义。
OBJECTIVE To establish a method for the simultaneous determination of 6-benzyladenine, prenyladenyl adenine, gibberellin, 4-fluorophenoxyacetic acid and 4-chlorobenzene in bean sprout by high performance liquid chromatography with self-made mixed solid phase extraction Oxyacetic acid method. Methods The samples were extracted with 20 ml of acetonitrile, purified by homemade SPE column, separated on a Spursil C18-EP column, acetonitrile and 0.5% phosphoric acid were used as the mobile phase and detected by UV detector. The detection wavelength was 209 nm. Standard method of quantitative. Results The five plant growth regulators were in the range of 0.5μg / ml ~ 50μg / ml with good linearity and the correlation coefficients were all> 0.999. The three concentrations of plant growth regulators (1 mg / kg, 10 mg / kg, 40 mg / ) As spiked, the average recoveries were 82.1% ~ 110.2%, and the relative standard deviations (RSDs) were all <6.5%. The limit of detection (S / N = 3) was 0.04 mg / kg ~ 0.10 mg / kg and the limit of quantitation (S / N = 10) was 0.06 mg / kg ~ 0.30 mg / kg. Conclusion Using homemade hybrid solid phase extraction column, sample processing is simple and quick. High-performance liquid chromatography simultaneous detection of five components, can ensure the accuracy, sensitivity, precision. Reduce time, personnel, environmental costs, for the absence of liquid chromatography-mass spectrometry associated grass-roots units in the detection of sprouts, has a certain promotion.