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    新型样品萃取瓶应用于高效液相色谱法测定卷烟爆珠壁材中的8种色素

    Determination of 8 Pigments in Wall Material of Cigarette Capsules by High Performance Liquid Chromatography with a Novel Sample Vial for Extraction

    • 摘要: 按GB 5606.1-2004的规定从一批卷烟中抽取卷烟样品,从每支卷烟的滤嘴中取出爆珠并剥取其壁材。称取此壁材0.200 0~0.300 0 g置于新型的样品萃取瓶的外套管中,加入水25 mL,并将萃取瓶的内套管卡在外套管中部,用密封圈予以固定。于70~80℃超声萃取35 min,待萃取瓶冷却至室温,将内套管向下压,使萃取液通过滤筛板过滤并通过内套管中的细弯管流出;收集经过滤的萃取液供高效液相色谱分析。采用Waters XBridge C18色谱柱为固定相,以不同比例的0.02 mol·L-1乙酸铵溶液和甲醇的混合液为流动相进行梯度洗脱,使样品中的8种色素得以分离。用二极管阵列检测器,在427 nm检测柠檬黄,在511 nm检测苋菜红、胭脂红、日落黄、诱惑红、酸性红及赤藓红,在625 nm检测亮蓝。此8种色素的质量浓度在一定范围内与其色谱峰面积之间呈线性关系,检出限(3S/N)在0.10~0.22 μg·g-1之间。加标回收率在93.2%~105%之间,测定值的日间和日内相对标准偏差(n=7)均小于5.0%。

       

      Abstract: Cigarettes of same batch were sampled as described in GB 5606.1-2004, and 0.200 0 to 0.300 0 g of the capsule shell, as stripped from the cigarette capsules in filter tips of each cigarette, was taken and placed into the outer case of the novel sample vial for extraction. 25 mL of water were added to the sample. The inner case of the extracting vial was then fixed at the mouth of the outer case with a sealing coil. The sample was extracted ultrasonically by keeping the extracting vial at 70 to 80℃ for 35 min. After cooling of the extracting vial to room temperature, the inner case was pressed downward to have the extract filtered though the dilter sieve plate, and the filtrate flowed out through the thin and curved tube in the inner case and was collected for use in HPLC analysis. Chromatographic separation of the 8 pigments in the sample was performed by using Waters XBridge C18 column as stationary phase, and mixtures of 0.02 mol·L-1 CH3COONH4 solution and methanol in various proportions as mobile phases in gradient elution. Diode array detector was used for detection. Tartrazine was detected at 427 nm, amaranth, cormine, sunset yellow, tempting red, acid red and red erythroplast were detected at 511 nm, and bright blue was detected at 625 nm. Linear relationships between values of mass concentrations of the 8 pigments and their corresponding peak areas were found in definite ranges, and the detection limits (3S/N) were in the range of 0.10 to 0.22 μg·g-1. Values of recovery obtained by standard addition method ranged from 93.2% to 105%, and values of intra-day and inter-day RSDs (n=7) were all less than 5.0%.

       

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