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目的建立自动顶空-气相色谱-质谱联用法(head space-gas chromatography-mass spectrometry,HS-GC-MS)检测食品纸包装材料中9种烯烃化合物(2-苯丙烯、苯丙烯、2-苯乙烯、二环[2,2,1]庚-2-烯、己烯、辛烯、异戊二烯、1,1-二氯乙烯和4-甲基-1-戊烯)的定性定量确证方法。方法样品在平衡温度为120℃,平衡时间为10 min的条件下自动顶空进样,经DB-624色谱柱分离,采用GC-MS选择离子扫描方式进行检测,以内标法定量。结果在优化的条件下,9种烯烃化合物在5~1000μg/kg范围内线性良好,相关系数(R~2)均大于0.999;方法定量限为20~40μg/kg;方法的回收率在93.5%~103.0%之间,相对标准偏差为2.3%~5.1%(n=6)。结论该方法简便准确,灵敏度高,重现性好,可满足食品纸包装材料中9种烯烃化合物检测的要求。
OBJECTIVE To establish an automated headspace-gas chromatography-mass spectrometry (HS-GC-MS) system for the determination of nine kinds of olefinic compounds (2-benzenepropylene, Qualitative and quantitative confirmation of ethylene, bicyclo [2,2,1] hept-2-ene, hexene, octene, isoprene, vinylidene chloride and 4-methyl- method. Methods The sample was automatically injected into the headspace at an equilibrium temperature of 120 ° C and an equilibration time of 10 min. The sample was separated on a DB-624 column and detected by GC-MS selective ionization. The internal standard method was used for quantification. Results Under the optimized conditions, the linearity of the nine alkene compounds was in the range of 5-1000 μg / kg, the correlation coefficients (R ~ 2) were all greater than 0.999. The limit of quantification was 20-40 μg / kg. The recovery was 93.5% ~ 103.0%, the relative standard deviation was 2.3% ~ 5.1% (n = 6). Conclusion The method is simple and accurate, high sensitivity and good reproducibility, which can meet the testing requirements of nine kinds of olefin compounds in food paper packaging materials.