HPLC法测定烟草及烟草制品中马来酰肼残留
Determination of Maleic Hydrazide Residue in Tobacco and Tobacco Products with High Performance Liquid Chromatography
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摘要: 建立了萃取溶剂、固相萃取小柱净化、高效液相色谱(HPLC)法检测烟草及烟草制品中马来酰肼(MH)残留量的方法,并采用该方法检测了23个烟草样品中的马来酰肼残留。结果表明:①用4 mol/L盐酸加热回流萃取1 h效果较好;②用Varian Microsorb-MV 100-5 C18色谱柱,以0.1 mol/L醋酸水溶液为流动相,等梯度洗脱,流速0.7 mL/min,检测波长313 nm,20 min内MH色谱峰和杂质色谱峰可以有效分离;③该法的回收率为97.11%,相对标准偏差为7.13%。该方法适合烟草及烟草制品中马来酰肼的测定。Abstract: A method for the determination of maleic hydrazide(MH)in tobacco and tobacco products was established, in which MH in tobacco sample was extracted with a solvent, and cleaned up by a solid phase extraction cartridge, then detected with high performance liquid chromatography. The residue of MH in 23 tobacco samples was determined. The results showed that: 1)Good results were obtainable when tobacco sample was extracted with 4 mol/L hydrochloric acid under heating and refluxing for 1 hour. 2)The MH peak was completely separated from impurity peaks in 20 minutes by reversed-phase HPLC with a Varian Microsorb-MV 100-5 C18 column under isocratic elution with 0.1 mol/L acetic acid as mobile phase at a flow-rate of 0.7 mL/min. 3)The recovery of MH was 97.11% with the relative standard deviation(RSD)of 7.13%. This method is suitable for the determination of MH in tobacco and tobacco products.
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