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GC-FID预测相对响应因子法测定卷烟爆珠中辛, 癸酸甘油酯含量

Quantification of octyl and decyl glycerate in flavor capsule for cigarette based on prediction of relative response factor by gas chromatography with flame ionization detector

  • 摘要: 为实现对混合物辛,癸酸甘油酯(ODO)的定量检测,建立了基于相对响应因子(RRF)的气相色谱-氢火焰离子化检测器(GC-FID)测定卷烟滤嘴爆珠中ODO含量(质量分数)的方法。1粒爆珠挤破后用正己烷提取,采用GC-FID检测,通过有效碳数(ECN)预测RRF,用内标法定量。结果表明:①采用该方法,ODO各组分分离效果良好,分析时间为20 min。②以三辛酸甘油酯或三癸酸甘油酯作为参考物质,在0~0.5 mg/mL范围内工作曲线的线性关系良好(R2>0.997),基于ODO总含量的加标回收率为98.0%~108.0%,相对标准偏差(RSD)≤ 2.0%,ODO各组分的定量限(LOQ)为0.05 mg/mL。③8个不同加香类型的实际卷烟爆珠样品中ODO含量为23%~87%,其中甘油三酯含量在ODO中占比在93%以上,甘油二酯占比在6%左右;采用两种参考物质的计算结果的一致性良好。该方法简单、高效,适用于卷烟爆珠中辛,癸酸甘油酯含量的测定。

     

    Abstract: For quantifying the total content of octyl and decyl glycerate (ODO) mixture in breakable flavor capsule for cigarette filter, a gas chromatography-flame ionization detector (GC-FID) method based on relative response factor principle was developed. One crashed capsule was vortex extracted with n-hexane, the components of ODO were analyzed by GC-FID. Based on the concept of effective carbon number (ECN), the relative response factor (RRF) for each component of ODO was estimated, and the quantification of total content of ODO mixture was achieved successfully by using caprylin or decanoin as calibration reference materials (RMs). The results showed that:1) Each component in ODO was well separated within 20 min. 2) Taking caprylin or decanoin as the calibration reference material, RMs had a good linear relationship (R2>0.997) in the range of 0-0.5 mg/mL. The recoveries of total content of ODO ranged from 98.0% to 108.0% with relative standard deviations no more than 2.0%. The LOQ of each component in ODO was 0.05 mg/mL. 3) The ODO content in breakable capsules in 8 commercial samples of different flavoring types was from 23% to 87%. Among the examined components in ODO, the highest component was triglyceride, which accounted for more than 93% of the total ODO content. The lowest component was diglyceride that accounted for about 6%. The ODO amount of all the samples quantified by using caprylin as the calibration reference material was consistent with that quantified by using decanoin. This method is simple, efficient and suitable for the determination of total content of ODO mixture in breakable capsules.

     

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