摘要
建立了气相色谱.质谱联用内标法测定干性食品包装纸中N.甲基吡咯烷酮的分析方法。采用超声提取为前处理方式,使用乙醇为溶剂,目标物用GC-MS进行了测定,内标法定量。探讨了不同萃取溶剂对目标物的提取效率,优选了合适的提取溶剂用量,比较了不同样品的提取方式及条件;甄选出合适的内标物,确定了较佳的特征离子及其丰度比,分析了色谱柱流量、进样量及分流比对目标物分离的影响,得到了合适的色谱分析条件。在优化的实验条件下.目标物N-甲基吡咯烷酮在0.02745。2.196mg/L范围内具有良好的线性关系,相关系数(R^2)为0.9999.平均回收率为98.36%~108.29%,相对标准偏差为3.71%~6.05%,检出限为0.058mg/kg,定量下限为0.194mg/kg。该方法简便、快速、灵敏、准确,适合于干性食品包装纸KN-甲基吡咯烷酮的测定。
A gas chromatography-mass spectrometry method (GC-MS) based on internal standard was developed for rapid determination of N-methyl pyrrolidone (NMP) in dry food wrappings. The NMP was extracted from the sample by ultrasonic extraction. The final product was determined by GC-MS based on internal standard. Extraction efficiency of different solvents on target object was discussed; suitable solvent dosage was determined; extraction modes and condi- tions for different samples were compared; suitable internal standard object was selected; the characteristic ions and its abundance were determined; the influence of column flow, injection volume, and split ratio on separation of target ob-ject was analyzed and suitable chromatography conditions were obtained. The result showed that under the optimal con- ditions, the calibration range of NMP was 0.02745 - 2. 196 mg/L with a correlation coefficient of 0. 9999 ; the average recoveries were in the range of 98.36% - 108.29% ; with relative standard deviations of 3.71% - 6.05%, the detec-tion limit and quantitation limit of NMP were 0. 058 mg/kg and 0. 194 mg/kg respectively. The method was simple, rapid, sensitive, accurate, and suitable for rapid determination of NMP in dry food wrappings.
出处
《包装工程》
CAS
CSCD
北大核心
2013年第21期6-11,共6页
Packaging Engineering