高级检索

    超高效液相色谱法测定烟草西柏三烯二醇

    Determination of Cembratriene-diol in Tobacco by Ultra Performance Liquid Chromatography

    • 摘要: 建立了超高效液相色谱-紫外检测(UPLC-UV)外标法定量测定烟草α和β-2,7,11-西柏三烯-4,6-二醇的方法。烟草样品以乙酸乙酯为萃取剂,液料比为50:1,在超声频率45 kHz,提取温度为25~30 ℃,提取时间10 min条件下进行目标化合物提取,提取液经氮气吹干,用流动相溶解,以ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7 µm)为分离色谱柱,以70%乙腈为流动相,流速为0.3 mL/min,柱温为35 ℃,在波长为200 nm条件下进行检测。结果表明,α和β-2,7,11-西柏三烯-4,6-二醇线性范围分别为12.14~194.2、6.229~99.67 μg/mL,仪器检出限分别为0.1166、0.1495 μg/mL,方法定量限分别为33.8、49.8 μg/g,在3个加标浓度下,平均回收率分别在96.7%~98.8%、96.2%~98.4 %,方法重现性相对标准偏差分别为3.46%、3.11%。本方法与行业标准相比,对烟草西柏三烯二醇的测定结果无显著差异。该方法操作简单、溶剂用量少,检测周期短,精密度和准确度均较高,适用于烟草α和β-2,7,11-西柏三烯-4,6-二醇批量检测。

       

      Abstract: A quantitative method using ultra performance liquid chromatography (UPLC) with UV detector was developed for the determination of α and β-2,7,11-Cembratriene-4,6-diol of tobacco.Ethyl acetate was used as solvent for extraction with a liquid-material ratio of 50:1.The ultrasonic frequency used was 45 kHz andthe temperature of extraction was room temperature above 25℃.The time of extraction was 10 min.The extracts obtained with above experiment conditions were dried by nitrogen and dissolved with mobile phases and the target compounds were separated on an ACQUITY UPLC BEH C18 column using acetonitrile-water (70:30) as mobile phase by gradient elution.The flow rate was set at 0.3 mL/min,the column temperature was 35℃ and quantitative wavelength of UV detector was set at 200 nm.The results indicated that the calibration curves of α and β-2,7,11-Cembratriene-4,6-dio were linear in the range of 12.14-194.2 μg/mLand 6.229-99.67 μg/mL respectively.The limits of detection (LOD,S/N=3) were 0.1166 and 0.1495 μg/mL respectively,and the limits of quantification (LOQ,S/N=10) were 33.8 μg/g and 49.8 μg/g respectively.The average recoveries of standard addition of samples were 96.7%-98.8% and 96.2%-98.4% respectively at three spiked concentration levels,and the relative standard deviations (RSDs) of reproducibility of the method were 3.46% and 3.11% respectively.There was no significant difference in the measurement results of tobacco samples between this method and the tobacco industry-standard method.The method was simple,sensitive and accurate,and was suitable for large scale determination of α and β-2,7,11-Cembratriene-4,6-dio in tobacco.

       

    /

    返回文章
    返回