食品用纸杯中光引发剂特定迁移量的气相色谱-串联质谱测定方法
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摘要
目的建立11种光引发剂类化合物食品用纸杯特定迁移量的气相色谱-串联质谱(gas chromatographytandem mass spectrometry,GC-MS/MS)检测方法。方法食品模拟物中的光引发剂类化合物经反相固相萃取柱富集净化后,采用中等级性的DM-17MS气相色谱柱进行分离;采用三重四极质谱的多反应监测模式(multiple reaction monitoring,MRM)对化合物进行定量测定。结果本方法可在17 min内完成11种目标化合物的色谱分离。11种光引发剂在低、中、高3个添加水平的回收率在65.0%~119.8%范围内,相对标准偏差为1.2%~10.6%(n=6),方法检出限为1~7μg/L,定量限为2~20μg/L。结论该方法灵敏度高,定量准确,适用于食品模拟物中光引发剂类物质特定迁移量的测定。
Objective To establish an analytical method for the determination of the migrants of 11 kinds of photoinitiator from paper cups into food simulants by gas chromatography-tandem mass spectrometric(GC-MS/MS). Methods The reverse-phased solid phase extraction cartridges were used for the extraction, enrichment and clean-up of the 11 kinds of potoinitiator from simulants. The analytes were separated on a moderately polar DM-17 MS column, and subsequently determined by triple quadruple mass spectrometry operating under multiple reaction monitor(MRM) mode. Results The GC-MS/MS analysis was achieved within 17 min. The recoveries of the method were ranged from 65.0% to 119.8% for the 11 kinds of photoinitiator at 3 spiked levels, and the relative standard deviations were between 1.2% and 10.6%. The limits of detection(LOD) and the limits of quantification(LOQ) were 1~7 μg/L and 2~20 μg/L, respectively. Conclusion The established method has been validated to be sensitive and accurate, which is applicable to the analysis of migrants of photoinitiators in food simulants.
Objective To establish an analytical method for the determination of the migrants of 11 kinds of photoinitiator from paper cups into food simulants by gas chromatography-tandem mass spectrometric(GC-MS/MS). Methods The reverse-phased solid phase extraction cartridges were used for the extraction, enrichment and clean-up of the 11 kinds of potoinitiator from simulants. The analytes were separated on a moderately polar DM-17 MS column, and subsequently determined by triple quadruple mass spectrometry operating under multiple reaction monitor(MRM) mode. Results The GC-MS/MS analysis was achieved within 17 min. The recoveries of the method were ranged from 65.0% to 119.8% for the 11 kinds of photoinitiator at 3 spiked levels, and the relative standard deviations were between 1.2% and 10.6%. The limits of detection(LOD) and the limits of quantification(LOQ) were 1~7 μg/L and 2~20 μg/L, respectively. Conclusion The established method has been validated to be sensitive and accurate, which is applicable to the analysis of migrants of photoinitiators in food simulants.
引文
[1]GB/T 27590-2011纸杯[S].GB/T 27590-2011 Paper cup[S].
[2]黄秀玲,王志伟,李明.影响PE淋膜纸中化学迁移物分配系数的因素[J].高分子材料科学与工程,2010,8(26):23-26.Huang XL,Wang ZW,Li M.Factors affecting partition coefficient of migrants from paper with PE coating[J].Poly Mater Sci Eng,2010,8(26):23-26.
[3]王晓芳,魏先福,黄蓓青.光引发剂对水性UV光油固化性能的影响[J].中国印刷与包装研究,2012,4(1):46-50.Wang XF,Wei XF,Huang BQ.Effect of photo-initiator on curing characteristics of water-based UV varnish[J].Chin Print Pack Study,2012,4(1):46-50.
[4]The EFSA.Opinion of the scientific panel of food additives,flavourings,processing aids and materials in contact with food on a request from the commission related to 2-isopropyl thioxanthone(ITX)and2-ethylhexyl-4-dimethylamino benzoate(EHDAB)in food contact materials[J].EFSA J,2005,293(12):1-15.
[5]邓晓军,郭德华,李波,等.气相色谱-质谱法测定乳制品中光引发剂异丙基硫杂蒽酮的残留量[J].色谱,2007,25(1):39-42.Deng XJ,Guo DH,Li B,et al.Determination of isopropylthioxanthone residue in milk migrated from packaging materials by gas chromatography-mass spectrometry[J].Chin J Chromatogr,2007,25(1):39-42.
[6]European Food Safety.EFSA statement on the presence of4-methylbenzophenone found in breakfast cereals[J].EFSA J,2009,243(3):1-19.
[7]Pastorelli S,Sanches-Silva A,Cruz JM,et al.Study of the migration of benzophenone from printed paperboard packages to cakes through different plastic films[J].Eur Food Res Technol,2008,227(6):1585-1590.
[8]Sanches-Silva A,Andre C,Castanheira I,et al.Study of the migration of photoinitiators used in printed food-packaging materials into food simulants[J].J Agric Food Chem,2009,57(20):9516-9523.
[9]Shen D,Lian HZ,Ding T,et al.Determination of low-level ink photoinitiator residues in packaged milk by solid-phase extraction and LC-ESI/MS/MS using triple-quadrupole mass analyzer[J].Anal Bioanal Chem,2009,395(7):2359-2370.
[10]韩伟,于艳军,李宁涛,等.食品接触材料表面印刷油墨中光引发剂的高效液相色谱-串联质谱法检测和迁移研究[J].分析化学,2011,39(9):1387-1393.Han W,Yu YJ,Li NT,et al.Determination and migration study of six photoinitiators in printing inks used for food contact materials by high performance liquid chromatography-tandem mass spectrometry[J].Chin J Anal Chem,2011,39(9):1387-1393.
[11]Hoeck EV,Schaetzen TD,Pacquet C,et al.Analysis of benzophenone and4-methylbenzophenone in breakfast cereals using ultrasonic extraction in combination with gas chromatography-tandem mass spectrometry(GC–MSn)[J].Anal Chim Acta,2010,663(1):55-59.
[12]张耀海,焦必宁,周志钦.气相色谱-串联质谱法结合Qu ECh ERS方法快速检测软包装饮料中8种光引发剂[J].分析化学,2012,40(10):1536-1542.Zhang YH,Jiao BN,Zhou ZQ.Analysis of eight photoinitiator residues in soft drinks using Qu ECh ERS method and gas chromatography-tandem mass spectrometric detection[J].Chin J Anal Chem,2012,40(10):1536-1542.
[13]刘芃岩,陈艳杰,赵春霞,等.固相微萃取-气相色谱/质谱法测定果汁及茶饮料中的10种光引发剂[J].色谱,2013,31(12):1232-1239Liu PY,Chen YJ,Zhao CX,et al.Determination of ten photoinitiators in fruit juices and tea beverages by solid-phase micro-extraction coupled with gas chromatography/mass spectrometry[J].Chin J Chromatogr,2013,31(12):1232-1239.
[14]李中皓,吴帅宾,刘珊珊,等.超高效合相色谱法快速检测纸质印刷包装材料中10种受限制光引发剂[J].分析化学,2013,41(12):1817-1824.Li ZH,Wu SB,Liu SS,et al.Rapid detection of ten restricted photoinitiators in paper-made packaging based on ultra performance convergence chromatography[J].Chin J Anal Chem,2013,41(12):1817-1824.
[15]GB 31604.1-2015食品安全国家标准食品接触材料及制品迁移试验通则[S].GB 31604.1-2015 National food safety standard,General principle for the migration experiments of food contact materials and products[S].
[16]GB/T 5009.156-2003食品用包装材料及其制品的浸泡试验方法通则[S].GB/T 5009.156-2003 General principle for the determination of migration of packaging materials and their products[S].
[2]黄秀玲,王志伟,李明.影响PE淋膜纸中化学迁移物分配系数的因素[J].高分子材料科学与工程,2010,8(26):23-26.Huang XL,Wang ZW,Li M.Factors affecting partition coefficient of migrants from paper with PE coating[J].Poly Mater Sci Eng,2010,8(26):23-26.
[3]王晓芳,魏先福,黄蓓青.光引发剂对水性UV光油固化性能的影响[J].中国印刷与包装研究,2012,4(1):46-50.Wang XF,Wei XF,Huang BQ.Effect of photo-initiator on curing characteristics of water-based UV varnish[J].Chin Print Pack Study,2012,4(1):46-50.
[4]The EFSA.Opinion of the scientific panel of food additives,flavourings,processing aids and materials in contact with food on a request from the commission related to 2-isopropyl thioxanthone(ITX)and2-ethylhexyl-4-dimethylamino benzoate(EHDAB)in food contact materials[J].EFSA J,2005,293(12):1-15.
[5]邓晓军,郭德华,李波,等.气相色谱-质谱法测定乳制品中光引发剂异丙基硫杂蒽酮的残留量[J].色谱,2007,25(1):39-42.Deng XJ,Guo DH,Li B,et al.Determination of isopropylthioxanthone residue in milk migrated from packaging materials by gas chromatography-mass spectrometry[J].Chin J Chromatogr,2007,25(1):39-42.
[6]European Food Safety.EFSA statement on the presence of4-methylbenzophenone found in breakfast cereals[J].EFSA J,2009,243(3):1-19.
[7]Pastorelli S,Sanches-Silva A,Cruz JM,et al.Study of the migration of benzophenone from printed paperboard packages to cakes through different plastic films[J].Eur Food Res Technol,2008,227(6):1585-1590.
[8]Sanches-Silva A,Andre C,Castanheira I,et al.Study of the migration of photoinitiators used in printed food-packaging materials into food simulants[J].J Agric Food Chem,2009,57(20):9516-9523.
[9]Shen D,Lian HZ,Ding T,et al.Determination of low-level ink photoinitiator residues in packaged milk by solid-phase extraction and LC-ESI/MS/MS using triple-quadrupole mass analyzer[J].Anal Bioanal Chem,2009,395(7):2359-2370.
[10]韩伟,于艳军,李宁涛,等.食品接触材料表面印刷油墨中光引发剂的高效液相色谱-串联质谱法检测和迁移研究[J].分析化学,2011,39(9):1387-1393.Han W,Yu YJ,Li NT,et al.Determination and migration study of six photoinitiators in printing inks used for food contact materials by high performance liquid chromatography-tandem mass spectrometry[J].Chin J Anal Chem,2011,39(9):1387-1393.
[11]Hoeck EV,Schaetzen TD,Pacquet C,et al.Analysis of benzophenone and4-methylbenzophenone in breakfast cereals using ultrasonic extraction in combination with gas chromatography-tandem mass spectrometry(GC–MSn)[J].Anal Chim Acta,2010,663(1):55-59.
[12]张耀海,焦必宁,周志钦.气相色谱-串联质谱法结合Qu ECh ERS方法快速检测软包装饮料中8种光引发剂[J].分析化学,2012,40(10):1536-1542.Zhang YH,Jiao BN,Zhou ZQ.Analysis of eight photoinitiator residues in soft drinks using Qu ECh ERS method and gas chromatography-tandem mass spectrometric detection[J].Chin J Anal Chem,2012,40(10):1536-1542.
[13]刘芃岩,陈艳杰,赵春霞,等.固相微萃取-气相色谱/质谱法测定果汁及茶饮料中的10种光引发剂[J].色谱,2013,31(12):1232-1239Liu PY,Chen YJ,Zhao CX,et al.Determination of ten photoinitiators in fruit juices and tea beverages by solid-phase micro-extraction coupled with gas chromatography/mass spectrometry[J].Chin J Chromatogr,2013,31(12):1232-1239.
[14]李中皓,吴帅宾,刘珊珊,等.超高效合相色谱法快速检测纸质印刷包装材料中10种受限制光引发剂[J].分析化学,2013,41(12):1817-1824.Li ZH,Wu SB,Liu SS,et al.Rapid detection of ten restricted photoinitiators in paper-made packaging based on ultra performance convergence chromatography[J].Chin J Anal Chem,2013,41(12):1817-1824.
[15]GB 31604.1-2015食品安全国家标准食品接触材料及制品迁移试验通则[S].GB 31604.1-2015 National food safety standard,General principle for the migration experiments of food contact materials and products[S].
[16]GB/T 5009.156-2003食品用包装材料及其制品的浸泡试验方法通则[S].GB/T 5009.156-2003 General principle for the determination of migration of packaging materials and their products[S].