超临界萃取-HPLC法检测烟叶中马来酰肼残留

Supercritical Extraction and HPLC Determination of Maleic Hydrazide from Pesticide Residues in Tobacco Leaves

用超临界CO2萃取烟叶中农残马来酰肼,用高效液相色谱检测马来酰肼残留量。通过单因素和正交实验对萃取过程中夹带剂、萃取压力、萃取温度、萃取时间和CO2流量进行了考察,确定了最佳萃取工艺条件为：夹带剂V（甲醇）∶V（异丙醇）=1∶1,萃取压力20 MPa,萃取温度55℃,萃取时间100 min,CO2流量23 g/min。在该条件下,采用高效液相色谱检测烟叶中马来酰肼残留量,分析的重现性和稳定性最佳。结果表明,马来酰肼回收率为94.08%-97.86%,RSD均小于6%,检出限为2.7μg/g。

Maleic hydrazide from tobacco leaves was extracted by supercritical carbon dioxide extraction and its content was determined by high performance liquid chromatography （HPLC）. The optimization of various extraction conditions like entrainers, extraction pressure, temperature, time and flow of carbon dioxide was investigated through single factor and orthogonal experiments, consecutively. The results showed that methanol and isopropanol with a volume ratio of 1：1 was the best entraine. And the optimization of extraction conditions was that extraction pressure was 20 MPa, extraction temperature was 55 ℃, extraction time was 100 min and flow of carbon dioxide was 23 g/min. The method developed here had excellent reproducibility and stability for the determination of maleic hydrazide in the extraction of tobacco leaves. Additionally, the recovery of this method were between 94. 08% and 97.86%, RSD was less than 6% , and detection limit maleic hydrazide was 2. 7μg/g.