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目的建立植物源性食品中多效唑、赤霉素、2,4-二氯苯氧乙酸、噻苯隆、氯吡脲、4-氯苯氧乙酸6种植物生长调节剂的超高效液相色谱-串联质谱测定方法。方法样品经Qu ECh ERS法进行预处理,选用含1%乙酸的乙腈溶液提取,十八烷基硅烷(C_(18))和无水硫酸镁粉末净化,采用BEH C_(18)(2.1 mm×100 mm,1.7μm)色谱柱为分离柱,以乙腈-0.1%氨水为流动相,梯度洗脱,流速为0.3 ml/min,柱温为35℃。除多效唑质谱检测条件为ESI+外,其余均为ESI-。结果 6种植物生长调节剂在测定浓度范围具有良好的线性关系(r≥0.999 0),各组分检出限:多效唑为0.05μg/kg;赤霉素和4-氯苯氧乙酸为1.0μg/kg;2,4-二氯苯氧乙酸和噻苯隆为0.5μg/kg;氯吡脲为0.1μg/kg。加标回收率为80.2%~115.8%,相对标准偏差为2.34%~5.20%。结论该方法操作简便,灵敏度和准确度均能满足植物源性食品中6种植物生长调节剂的检测要求。
OBJECTIVE To establish a method for the determination of six plant growth regulators of plant-derived food including paclobutrazol, gibberellin, 2,4-dichlorophenoxyacetic acid, thidiazuron, clopidogrel and 4-chlorophenoxyacetic acid by ultra performance liquid chromatography- Tandem mass spectrometry method. Methods The samples were pretreated by Qu ECh ERS method. The samples were extracted with acetonitrile containing 1% acetic acid, and purified with octadecylsilane (C_ (18)) and anhydrous magnesium sulfate powders. The samples were eluted with BEH C 18 100 mm, 1.7 μm) was used as the separation column. The mobile phase consisted of acetonitrile-0.1% aqueous ammonia with gradient elution at a flow rate of 0.3 ml / min and a column temperature of 35 ℃. In addition to the detection conditions for paclobutrazol mass spectrometry ESI +, the rest are ESI-. Results Six plant growth regulators had a good linear relationship (r≥0.999 0) in the range of determination concentration. The detection limits of each component were as follows: paclobutrazol 0.05μg / kg; gibberellin and 4-chlorophenoxyacetic acid 1.0μg / kg; 2,4-Dichlorophenoxyacetic acid and thidiazuron were 0.5 μg / kg; and Chlorpheniramine was 0.1 μg / kg. The spiked recoveries ranged from 80.2% to 115.8% with relative standard deviations of 2.34% -5.20%. Conclusion The method is simple, sensitive and accurate to meet the detection requirements of six plant growth regulators in plant-derived foods.