手性色谱柱-HPLC-DAD法分离分析烟草与烟草制品中烟碱旋光异构体
Separation and analysis of nicotine enantiomers in tobacco and tobacco products using chiral column-HPLC-DAD method
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摘要: 选用大赛璐手性色谱柱CHIRALPAK-IC,以V(正己烷): V(异丙醇)=95:5的混合溶液为流动相,以二乙胺为流动相添加剂,在正相色谱模式下,建立了手性色谱柱-高效液相色谱-二极管阵列检测器法(HPLC-DAD)分离分析烟草与烟草制品中烟碱旋光异构体.对该方法的表征和检验结果表明:1)左旋烟碱和右旋烟碱分别在15~750 μg/mL,0.75~30.00 μg/mL质量浓度范围内线性关系良好,二者检出限和定量限分别为0.02 mg/g和0.05 mg/g;2)烟碱的日内、日间测定结果的精密度分别小于等于0.85%,4.00%;左旋烟碱和右旋烟碱的回收率分别为94.93%~103.70%,92.50%~117.50%.这表明本方法精密度较好,回收率较高.使用该方法对26个不同类型烟草及烟草制品的烟碱旋光异构体进行测定发现,烟草中主要为左旋烟碱,仅6个样品中检出右旋烟碱,且右旋烟碱质量占总烟碱比例为0.18%~0.70%;10个成品卷烟烟丝及其主流烟气中,右旋烟碱质量占总烟碱的比例明显高于卷烟烟丝.Abstract: The CHIRALPAK-IC was used, and the mixed solution of V (n-hexane):V (isopropanol)=95:5 was used as the mobile phase, and diethylamine was used as the mobile phase additive. In normal phase chromatography mode, a chiral column-high performance liquid chromatography-diode array detector (HPLC-DAD) method was developed for the separation and analysis of nicotine optical isomers in tobacco and tobacco products. The characterization and test results of this method indicated:1) The linear relationship between S-(-)-nicotine and R-(+)-nicotine was in the range of 15~750 μg/mL and 0.75~30.00 μg/mL, respectively. The detection limit and limit of quantification were 0.02 mg/g and 0.05 mg/g, respectively. 2)The precision of intra-and inter-day measurements of nicotine was less than 0.85% and 4.00%, respectively; the recovery rates of S-(-)-nicotine and R-(+)-nicotine were 94.93%~103.70% and 92.50%~117.50%, respectively. This indicated that the method had good precision and high recovery rate. Using this method to determine the nicotine optical isomers of 26 different types of tobacco and tobacco products, it was found that tobacco was mainly S-(-)-nicotine, only 6 samples were detected by R-(+)-nicotine. The proportion of nicotine quality was 0.18%~0.70%; among the 10 finished cigarettes and their mainstream smoke, the proportion of R-(+)-nicotine in total cigarette smoke was higher than that of cigarette tobacco.
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Key words:
- tobacco /
- tobacco product /
- chiral column /
- HPLC-DAD /
- nicotine enantiomers
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