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目的建立豆芽中2,4-D、2,4-D丁酯、4-氯苯氧乙酸、吲哚乙酸、吲哚丁酸、萘乙酸的气相色谱-质谱法(GC-MS)。方法使用酸化乙腈为提取液,浓缩干燥后加入2 ml甲醇溶解,取其中1 ml经Qu ECHERS试剂盒净化后测定2,4-D丁酯;另外1 ml甲醇样液经MCS固相萃取柱净化后,用10%三氟化硼甲醇溶液甲酯化,提取后GC-MS测定其余5种植物生长调节剂。结果 6种植物生长调节剂在0.5μg/ml~5.0μg/ml质量浓度范围内呈良好的线性关系,相关系数为0.991 0~0.999 3。在空白样品中分别添加浓度为0.5μg/ml和2.0μg/ml的标准溶液,平均回收率为79.8%~89.9%,相对标准偏差(RSD)为3.9%~9.1%。结论本方法简单、快速、可靠,结合Qu ECHERS净化法可以满足豆芽中植物生长调节剂多残留检测的要求。
Objective To establish a gas chromatography-mass spectrometry (GC-MS) method for determination of 2,4-D, 2,4-D butyl ester, 4-chlorophenoxyacetic acid, indole acetic acid, indole butyric acid and naphthalene acetic acid in bean sprouts. Methods Acidified acetonitrile was used as the extract. After concentrated and dried, 2 ml of methanol was added for dissolving. One ml was purified by Qu ECHERS kit to determine 2,4-D butyl ester. Another 1 ml of methanol was purified by MCS column After methyl esterification with 10% boron trifluoride methanol solution, the remaining five plant growth regulators were determined by GC-MS after extraction. Results Six plant growth regulators showed good linearity in the range of 0.5μg / ml ~ 5.0μg / ml with the correlation coefficient of 0.991 0 ~ 0.999 3. The standard solutions with the concentration of 0.5μg / ml and 2.0μg / ml were respectively added to the blank samples. The average recoveries were 79.8% ~ 89.9% with relative standard deviations (RSDs) of 3.9% ~ 9.1%. Conclusion The method is simple, rapid and reliable, and combined with Qu ECHERS purification method can meet the requirements of multi-residue detection of plant growth regulator in bean sprouts.