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

作　　者：赵旦 祖铁红 纪欣欣 黄学者 贾光群 李岩[1] 崔宗岩 ZHAO Dan;ZU Tie-Hong;JI Xin-Xin;HUANG Xue-Zhe;JIA Guang-Qun;LI Yan;CUI Zong-Yan(College of Environmental and Chemical Engineering,Yanshan University,Qinhuangdao 066004,China;Technology Center of Qinhuangdao Customs,Qinhuangdao 066004,China)

机构地区：[1]燕山大学环境与化学工程学院,秦皇岛066004 [2]秦皇岛海关技术中心,秦皇岛066004

出　　处：《食品安全质量检测学报》2024年第19期197-203,共7页Journal of Food Safety and Quality

基　　金：海关总署科研项目(2022HK023)。

摘　　要：目的建立固相萃取结合气相色谱-质谱法(gas chromatography-massspectrometry,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,利用亲水亲脂平衡(hydrophilic lipophilic balanced,HLB)固相萃取柱对3-氰基吡啶富集净化,DM-Wax色谱柱(50 m×250μm,0.5μm)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0.1~10.0 mg/L质量浓度范围内线性良好(R^(2)=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 3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)。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。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。Objective To establish an analytical method for the determination of 3-cyanopyridine in honey by solid phase extraction coupled with gas chromatography-mass spectrometry(GC-MS).Methods Honey samples were dissolved in deionized water and then 3-cyanopyridine was enriched and purified by hydrophilic lipophilic balanced(HLB)solid phase extraction column,separated by DM-Wax column(50 m×250μm,0.5μm),detected by selective ion monitoring mode,and quantified by external standard method.Results The linearity(R^(2)=0.9999)of 3-cyanopyridine was good in the concentration range of 0.1-10.0 mg/L,the limit of detection and the limit of quantitation 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 of the method ranged from 93.7%to 100.2%,and the relative standard deviations were 2.3%-5.4%(n=6).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 content was near the limit of quantitation,and all≤0.15 mg/kg,which was far lower than the content of jujube honey.Conclusion The method is simple,sensitive and accurate,and is suitable for the determination of 3-cyanopyridine in honey.

关 键 词：枣花蜂蜜 3-氰基吡啶 气相色谱-质谱法 固相萃取 

分 类 号：S896.1[农业科学—特种经济动物饲养] O657.63[农业科学—畜牧兽医]