气相色谱-串联质谱法测定大米中非法添加的石蜡
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摘要
建立测定大米中石蜡的气相色谱-串联质谱(GC-MS/MS)法。样品经石油醚提取,浓缩后用正己烷溶解,加浓硫酸净化,通过对C_(24)、C_(26)、C_(28)、C_(30)、C_(33)5种烷烃的测定,进行石蜡的定性分析,用上述5种烷烃的峰面积之和进行定量分析。该方法的检出限为0.25mg/kg,定量限为0.75mg/kg,加标回收率及精密度实验的平均回收率为93.38%～110.22%,相对标准偏差(RSD)为5.42%～12.11%,相关系数为0.9980。结果表明,该方法精密度良好,检测结果可靠,可作为大米中石蜡的测定方法。
A method for the determination of paraffin in rice by GC-MS/MS was established. The samples were extracted with petroleum ether, condensed, dissolved with n-hexane, and purified by concentrated sulfuric acid. The paraffin was qualitatively analyzed by the determination of 5 alkanes including C_(24), C_(26), C_(28), C_(30) and C_(33), and quantitatively analyzed by the sum of the peak area of 5 alkanes. The detection limit of the method was 0.25 mg/kg,and the limit of quantitation was 0.75 mg/kg, the standard recovery rate and the average recovery rate of the precision experiments were 93.38%-110.22%,the relative standard deviation(RSD) was 5.42%-12.11%, and the correlation coefficient was 0.9980. The results showed that the precision of the method was good, the results were reliable, and the method could be used for the determination of paraffin in rice.
A method for the determination of paraffin in rice by GC-MS/MS was established. The samples were extracted with petroleum ether, condensed, dissolved with n-hexane, and purified by concentrated sulfuric acid. The paraffin was qualitatively analyzed by the determination of 5 alkanes including C_(24), C_(26), C_(28), C_(30) and C_(33), and quantitatively analyzed by the sum of the peak area of 5 alkanes. The detection limit of the method was 0.25 mg/kg,and the limit of quantitation was 0.75 mg/kg, the standard recovery rate and the average recovery rate of the precision experiments were 93.38%-110.22%,the relative standard deviation(RSD) was 5.42%-12.11%, and the correlation coefficient was 0.9980. The results showed that the precision of the method was good, the results were reliable, and the method could be used for the determination of paraffin in rice.
引文
[1]中华人民共和国国家卫生和计划生育委员会.GB 2760-2014食品安全国家标准食品添加剂使用标准[S].北京:中国标准出版社,2014.
[2]毕艳兰,范璐.涂石蜡大米石蜡含量定量方法研究[J].食品科学,2006,27(7):202-204.
[3]曲海波.顶空气相色谱法测定石蜡中微量苯和甲苯[J].当代化工,2004,33(3):197-198.
[4]中华人民共和国国家质量监督检验检疫总局.GB/T 21309-2007涂渍油脂或石蜡大米检验[S].北京:中国标准出版社,2007.
[5]孙晓燕.对测定食用油掺入矿物油的几种方法的探讨[J].粮油仓储科技通讯,2008,24(2):47-48.
[6]郑卫东,周燕,钟红霞,等.火锅底料中石蜡的定性检验[J].中国测试,2005,31(5):85-86.
[7]廖怀平,蔡元庠,肖伦.傅里叶红外光谱法检测火锅底料中的固体石蜡[J].中国卫生检验杂志,2005,15(12):1456-1457.
[8]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),2008,44(7):653-654.
[9]SIMAL-GáNDARA J,SARRIA-VADAL M,RIJK R.Determination of paraffins in food simulants and packaging materials by liquid chromatography with evaporative mass detection and identification of paraffin type by liquid chromatography/gas chromatography and fourier transform infrared spectroscopy[J].J Aoac Int,2000,83(2):311-319.
[10]FISELIER K,FIORINI D,GROB K.Activated aluminum oxide selectively retaining long chain n-alkanes.Part II.Integration into an on-line HPLC-LC-GC-FID method to remove plant paraffins for the determination of mineral paraffins in foods and Environmental samples[J].Anal Chim Acta,2009,634(1):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,2009,37(12):1765-1770.
[12]张玉,蔡铮,王伟,等.气相色谱法测定香菇中石蜡的含量[J].浙江农业科学,2012,1(6):870-872.
[13]NILSSON M L,BENGTSSON S,KYLIN H.Identification and determination of chlorinated paraffins using multivariate evaluation of gas chromatographic data[J].Environ Pollut,2012,163:142-148.
[14]杨军,胡飞杰,胡文彦,等.气相及气相色谱质谱法测定食品中非法添加的石蜡[J].安徽农业科学,2011,39(29):18226-18228.
[15]吴泽君,谢佳琦,郭世明,等.红薯粉条中非法添加物石蜡指标性成分的检测方法研究[J].食品工业科技,2017,38(3):290-294.
[16]STEJNAROVáP,COELHAN M,KOSTRHOUNOVáR,et al.Analysis of short chain chlorinated paraffins in sediment samples from the Czech Republic by short-column GC/ECNI-MS[J].Chemosphere,2005,58(3):253-262.
[17]刘飞.食用菌中石蜡的气相色谱/质谱联用法测定[J].食品研究与开发,2010,31(12):133-135.
[18]韦迪哲,王蒙,姜楠,等.气相色谱/质谱法测定打蜡脐橙的石蜡含量[J].食品安全质量检测学报,2016,7(2):523-528.
[19]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(1):165-169.
[20]沈涛,秦炬,孙颖霞,等.凝胶渗透色谱-气相色谱/质谱法测定瓜子中的石蜡含量[J].安徽农业科学,2012,40(14):8223-8224.
[2]毕艳兰,范璐.涂石蜡大米石蜡含量定量方法研究[J].食品科学,2006,27(7):202-204.
[3]曲海波.顶空气相色谱法测定石蜡中微量苯和甲苯[J].当代化工,2004,33(3):197-198.
[4]中华人民共和国国家质量监督检验检疫总局.GB/T 21309-2007涂渍油脂或石蜡大米检验[S].北京:中国标准出版社,2007.
[5]孙晓燕.对测定食用油掺入矿物油的几种方法的探讨[J].粮油仓储科技通讯,2008,24(2):47-48.
[6]郑卫东,周燕,钟红霞,等.火锅底料中石蜡的定性检验[J].中国测试,2005,31(5):85-86.
[7]廖怀平,蔡元庠,肖伦.傅里叶红外光谱法检测火锅底料中的固体石蜡[J].中国卫生检验杂志,2005,15(12):1456-1457.
[8]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),2008,44(7):653-654.
[9]SIMAL-GáNDARA J,SARRIA-VADAL M,RIJK R.Determination of paraffins in food simulants and packaging materials by liquid chromatography with evaporative mass detection and identification of paraffin type by liquid chromatography/gas chromatography and fourier transform infrared spectroscopy[J].J Aoac Int,2000,83(2):311-319.
[10]FISELIER K,FIORINI D,GROB K.Activated aluminum oxide selectively retaining long chain n-alkanes.Part II.Integration into an on-line HPLC-LC-GC-FID method to remove plant paraffins for the determination of mineral paraffins in foods and Environmental samples[J].Anal Chim Acta,2009,634(1):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,2009,37(12):1765-1770.
[12]张玉,蔡铮,王伟,等.气相色谱法测定香菇中石蜡的含量[J].浙江农业科学,2012,1(6):870-872.
[13]NILSSON M L,BENGTSSON S,KYLIN H.Identification and determination of chlorinated paraffins using multivariate evaluation of gas chromatographic data[J].Environ Pollut,2012,163:142-148.
[14]杨军,胡飞杰,胡文彦,等.气相及气相色谱质谱法测定食品中非法添加的石蜡[J].安徽农业科学,2011,39(29):18226-18228.
[15]吴泽君,谢佳琦,郭世明,等.红薯粉条中非法添加物石蜡指标性成分的检测方法研究[J].食品工业科技,2017,38(3):290-294.
[16]STEJNAROVáP,COELHAN M,KOSTRHOUNOVáR,et al.Analysis of short chain chlorinated paraffins in sediment samples from the Czech Republic by short-column GC/ECNI-MS[J].Chemosphere,2005,58(3):253-262.
[17]刘飞.食用菌中石蜡的气相色谱/质谱联用法测定[J].食品研究与开发,2010,31(12):133-135.
[18]韦迪哲,王蒙,姜楠,等.气相色谱/质谱法测定打蜡脐橙的石蜡含量[J].食品安全质量检测学报,2016,7(2):523-528.
[19]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(1):165-169.
[20]沈涛,秦炬,孙颖霞,等.凝胶渗透色谱-气相色谱/质谱法测定瓜子中的石蜡含量[J].安徽农业科学,2012,40(14):8223-8224.