Study on determination of paraffin's index components illegally added into sweet potato vermicelli
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摘要: 建立了气相色谱法（GC）及气相色谱质谱法（GC-MS）测定红薯粉条中非法添加物石蜡指标性成分正二十二烷和正二十八烷的方法。样品经湿法消解,石油醚（3060℃）萃取,旋转蒸发至干,正己烷定容后进样GC及GC-MS分析。GC法正二十二烷回收率为80.7%82.5%,相对标准偏差为8.2%9.9%,检出限为2.4 mg/kg,定量限为3.8 mg/kg;正二十八烷回收率为83.4%86.2%,相对标准偏差为7.8%9.3%,检出限为1.8 mg/kg,定量限为3.3 mg/kg,GC-MS法正二十二烷回收率为81.1%84.5%,相对标准偏差为7.2%9.8%,检出限为0.1 mg/kg,定量限为0.2 mg/kg;正二十八烷回收率为80.0%86.7%,相对标准偏差为6.5%9.2%,检出限为0.05 mg/kg,定量限为0.07 mg/kg。GC-MS较GC专属性强,灵敏度高,定量准确,能满足于红薯粉条中非法添加的石蜡的检测。Abstract: Two methods,gas chromatography( GC) and gas chromatography- mass spectrometry( GC- MS) were proposed for the determination of n- Docosane and n- Octacosane,which were the index components of paraffin illegally added into sweet potato vermicelli.After wet digestion,extracted with petroleum ether( b.p 30~60 ℃),the samples were drying with rotary evaporation.Subsequently,the analytes were analyzed by GC and GC- MS after dissolved with n- hexane.The recoveries of n- Docosane and n- Octacosane in GC method were 80.7% ~82.5% and 83.4% ~86.2%,respectively,with the relative standard deviations 8.2%~9.9% and 7.8% ~9.3%,while those of GC- MS method were 81.1% ~84.5% and 80.0% ~86.7%,and the relative standard deviations were 7.2% ~9.8% and 6.5% ~9.2%,respectively. The limit of detection( LOD) and the limit of quantitation( LOQ)about n- Docosane were 2.4 mg / kg and 3.8 mg / kg separately in GC,while those of n- Octacosane were 1.8 mg / kg and3.3 mg / kg. In GC- MS,the LOD and LOQ of n- Docosane were 0.1 mg / kg and 0.2 mg / kg,while those of n- Octacosane were0.05 mg / kg and 0.07 mg / kg separately.Compared with GC,GC- MS had a better performance about specificity,sensitivity and quantification,and this method was suitable for the detection of paraffin added illegally in sweet potato vermicelli.
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[1] 范璐,毕艳兰,蔡凤英.涂石蜡大米的石蜡含量测定方法的研究[J].中国粮油学报,2006,21(4):131-134. [2] 中华人民共和国国家质量监督检验检疫总局.GB/T21309-2007涂渍油脂或石蜡大米检验法[S].北京:中国标准出版社,2007. [3] 中华人民共和国国家质量监督检验检疫总局.GB/T24313-2009蜂蜡中石蜡的测定气相色谱-质谱法[S].北京:中国标准出版社,2009. [4] 周颖,陈亚林,张学煃.傅里叶变换红外光谱法检测火锅用牛油中固体石蜡[J].理化检验(化学分册),2008,4(7):653-657. [5] 王亚琴,祝红昆,李军明,等.火锅底料中石蜡检测的样品前处理研究[J].现代仪器与医疗,2013,19(1):73-73. [6] Louise M M,Pim EG L,Caroline G,et al.Recent developments in capabilities for analysing chlorinated paraffins in environmental matrices:A review[J].Chemosphere,2015,136:259-272.
[7] 孙力军,徐枫,李仁伟,等.气相色谱-质谱联用法测定大米中的石蜡[J].食品研究与开发,2013,34(18):58-61. [8] Nilsson M-L,Staffan B,Henrik K.Identification and determination of chlorinated paraffins using multivariate evaluation of gas chromatographic data[J].Environmental Pollution,2012,163:142-148.
[9] 吴玉銮,陈意光,罗东辉,等.氧化除杂-气相色谱/质谱联用测定食品中的石蜡[J].现代食品科技,2014,30(1):165-169. [10] Katell F,Dennis F,Koni G.Activated aluminum oxide selectively retaining long chain n-alkanes:Part II.Integration into an on-line high performance liquid chromatography-liquid chromatography-gas chromatography-flame ionization detection method to remove plant paraffins for the determination of mineral paraffins in foods and environmental samples[J].Analytica Chimica Acta,2009,634:102-109.
[11] 盛旋,胡艳云,张蕾,等.正相液相色谱-蒸发光散射法测定食品中的石蜡[J].分析化学,2009,12(32):1765-1770.
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