固相萃取-气相色谱-质谱法测定蜂蜜中的3-氰基吡啶

Determination of 3-cyanopyridine in honey by solid phase extraction-gas chromatography-mass spectrometry

中文关键词:  枣花蜂蜜  3-氰基吡啶  气相色谱质谱法  固相萃取

英文关键词:jujube honey  3-cyanopyridine  gas chromatography-mass spectrometry  solid phase extraction

中文摘要:

      目的 建立一种利用气相色谱-质谱法(gas chromatography-mass spectrometry，GC-MS)测定蜂蜜中3-氰基吡啶的分析方法。方法 蜂蜜样品经去离子水溶解后,利用HLB固相萃取柱对3-氰基吡啶富集净化,DM-Wax色谱柱(50 m×250 μm×0.5 μm)分离,采用选择离子监测模式检测,外标法定量。结果 3-氰基吡啶在0.1~10 mg/L浓度范围内线性良好(R₂^=0.9999),方法检出限和定量限分别为0.04 mg/kg和0.12 mg/kg,在0.12、0.24、1.20 mg/kg三个添加浓度水平下,平均回收率范围为93.7%~100.2%,相对标准偏差范围为2.3%~5.4%(n=6)。结论 该方法操作简便,灵敏度高,准确性好,适用于蜂蜜中3-氰基吡啶的测定。应用建立的方法对不同蜜源植物的蜂蜜样品进行检测,发现枣花蜂蜜中均检出较高含量的3-氰基吡啶(0.40~2.25 mg/kg),在油菜、椴树、荔枝、荆条、洋槐蜂蜜中也检出一定含量的3-氰基吡啶,但其含量多在定量限附近,且均≤0.15 mg/kg,远低于枣花蜂蜜。因此,高含量3-氰基吡啶可作为潜在特征指标用于鉴别枣花蜂蜜。

英文摘要:

      To establish an analytical method for the determination of 3-cyanopyridine in honey by gas chromatography-mass spectrometry (GC-MS). Methods Honey samples were dissolved in deionized water and then 3-cyanopyridine was enriched and purified by HLB solid phase extraction column, separated by DM-Wax column (50 m×250 μm×0.5 μm), detected by selective ion monitoring mode, and quantified by external standard method. Results The linearity (R2=0.9999) of 3-cyanopyridine was good in the concentration range of 0.1~10 mg/L, the limit of detection and the limit of quantitative of the method were 0.04 mg/kg and 0.12 mg/kg, respectively. At the spiked levels of 0.12, 0.24 and 1.20 mg/kg, the average recoveries rate of the method ranged from 93.7% to 100.2%, and the relative standard deviation was 2.3%~5.4%. Conclusion The method is simple, sensitive and accurate, and is suitable for the determination of 3-cyanopyridine in honey. The established method was applied to detect honey samples which from different nectar plants, and it was found that high content of 3-cyanopyridine (0.40~2.25 mg/kg) was detected in jujube honey. Although a certain amount of 3-cyanopyridine was also detected in rape, linden, litchi, vitex and acacia honey, most of its contents were near the limit of quantitative, and all were ≤0.15 mg/kg, which was far lower than the content of jujube honey. Therefore, high content of 3-cyanopyridine could be used as a latent characteristic index to identify jujube honey.