低温粉碎结合超声萃取-气相色谱-质谱联用法测定高分子抗菌食品包装材料中4种抗菌剂的残留量

Determination of 4 kinds of antimicrobials in polymeric antimicrobial food-packaging materials by cryogenic comminution and ultrasonic extraction tandem with gas chromatography-mass spectrometry

中文关键词:  气相色谱质谱联用法  高分子抗菌食品包装材料  抗菌剂  残留

英文关键词:gas chromatography-mass spectrometry  polymeric antimicrobial food-packaging materials  antimicrobial agent  residues

中文摘要:

      目的 建立低温粉碎结合超声萃取-气相色谱-质谱联用法测定高分子食品包装材料中二苯基醚、4,4’-二甲基二苯醚、4,4’-二羟基二苯醚、三氯生等4种抗菌剂残留量的分析方法。方法 样品经液氮冷冻粉碎后, 通过采用丙酮-二氯甲烷混合溶液超声萃取, DB-5ms色谱柱分离, 气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)选择离子扫描模式(SIM)检测以及外标法定量来进行检测分析。结果 当丙酮-二氯甲烷混合溶液的配比为3:7 (V:V)时, 结果最佳。在优化条件下检测, 4种抗菌剂在0.2~10 mg/L范围内线性良好, 线性相关系数大于0.99, 回收率为84.7%~104.7%, 相对标准偏差RSD为3.2%~12.9%, 方法定量限为2.0 mg/kg。结论 该方法简便、快捷、准确, 适合对高分子食品包装材料中二苯基醚、4,4’-二甲基二苯醚、4,4’-二羟基二苯醚、三氯生残留量进行检测分析。

英文摘要:

      Objective To establish a method for determination of 4 kinds of antimicrobials (diphenyl ether, 4,4'-dimethydiphenyl ether, 4,4'-oxydiphenol and triclosan) in polymeric antimicrobial food-packaging materials by cryogenic comminution and ultrasonic extraction tandem with gas chromatography-mass spectrometry (GC-MS). Methods Samples were freezing-smashed with liquid nitrogen, extracted by mixed solvents of acetone and dichloromethane with ultrasonic, separated by DB-5ms column, detected by GC-MS, and quantitated by external standard method. Results The best optimal proportion of acetone and dichloromethane was 3:7 (V:V). Under optimized conditions, a good linear of 4 antimicrobial were showed between 0.2~10 mg/L, with correlation coefficients (r) above 0.99. The recoveries were ranged from 84.7% to 104.7%, the relative standard deviations (RSDs) were between 3.2%~12.9%, and the limits of quantization (LOQ) were 2.0 mg/kg. Conclusion The proposed method is rapid, accurate and sensitive, which is suitable for detecting diphenyl ether, 4,4'-dimethydiphenyl ether, 4,4'-oxydiphenol and triclosan in polymeric antimicrobial food-packaging materials.