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目的建立气相色谱-质谱法测定豆芽中的7种植物生长调节剂残留量的方法。方法样品经组织捣碎、乙腈提取、甲醇定容后,采用GC-MS检测2,4-D-乙酯和2,4-D-丁酯;另取甲醇定容液1 ml,经QuEChERS净化、MCS柱过滤、三氟化硼甲醇进行衍生后,采用GC-MS检测4-氯苯氧乙酸、2,4-二氯苯氧乙酸(2,4-D)、α-萘乙酸、吲哚乙酸和吲哚丁酸。结果 7种植物生长调节剂在0.5μg/ml~10μg/ml时具有良好的线性关系,相关系数(r)均≥0.991 5。7种植物生长调节剂的LOD为0.01 mg/kg,LOQ为0.03 mg/kg,平均加标回收率为92.2%~97.4%,相对标准偏差(RSD)为4.8%~10.1%。276份豆芽样品中,4-氯苯氧乙酸检出93份,吲哚乙酸检出70份,吲哚丁酸检出26份;2,4-D、2,4-D-乙酯、α-萘乙酸和2,4-D-丁酯4个指标在所有豆芽样品中均未检出。结论该方法灵敏度高,回收率高,检测限低,符合分析要求,适合豆芽中7种植物生长调节剂残留检测的要求。
Objective To establish a method for the determination of 7 plant growth regulators in bean sprouts by gas chromatography-mass spectrometry. Methods The samples were mashed by tissue, extracted with acetonitrile and fixed in methanol. The contents of 2,4-D-ethyl ester and 2,4-D-butyl ester were determined by GC-MS. , MCS column filtration, boron trifluoride methanol derivatization, GC-MS detection of 4-chlorophenoxyacetic acid, 2,4-dichlorophenoxyacetic acid (2,4-D), α-naphthalene acetic acid, indole Acetic acid and indole butyric acid. Results Seven plant growth regulators had a good linear relationship at 0.5μg / ml ~ 10μg / ml with correlation coefficients (r) ≥0.991. The LOD of 5.7 kinds of plant growth regulators was 0.01 mg / kg and the LOQ was 0.03 mg / kg. The average recoveries were 92.2% -97.4% with relative standard deviations (RSDs) of 4.8% -10.1%. Among the 276 sprouts samples, 93 were detected by 4-chlorophenoxyacetic acid, 70 were detected by indole acetic acid and 26 were detected by indole butyric acid. 2,4-D, 2,4-D-ethyl ester, α - naphthalene acetic acid and 2,4-D-butyl ester four indicators were not detected in all samples of bean sprouts. Conclusion The method has high sensitivity, high recovery and low detection limit, which meets the analytical requirements and is suitable for the detection of 7 kinds of plant growth regulators residues in bean sprouts.