超高效液相色谱-串联质谱法测定食品接触材料中油酸酰胺的迁移量
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摘要
目的 建立超高效液相色谱-串联质谱法测定食品接触材料中油酸酰胺迁移量的分析方法。方法 按照GB 5009.156-2016《食品安全国家标准食品接触材料及制品迁移试验预处理方法通则》的要求配制5种食品模拟液,幵按照标准要求迚行浸泡试验,浸泡液经过滤后迚样,经过ZORBAX C_18(3.0mm×100mm,1.8μm)色谱柱分离,在正离子模式下以电喷雾电离多反应监测模式迚行定性和定量分析。结果 5种食品模拟物(4%乙酸、10%乙醇、20%乙醇、50%乙醇以及95%乙醇)中的油酸酰胺在0.25～5.0 mg/L浓度范围具有较好线性,相关系数(r2)均大于0.9990,方法检出限为0.001～0.002mg/L,方法定量限为0.003～0.005mg/L,油酸酰胺在3个浓度水平的加标回收率为90.3%～117.1%,相对标准偏差为0.20%～2.10%(n=6)。结论 该方法灵敏、准确,能够满足食品接触材料中油酸酰胺的迁移量的检测。
Objective To establish a method for the determination of oleamide migration from food contact materials by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods According to the GB5009.156-2016 National food safety standards-Food contact materials and products migration test pretreatment methods, 5 kinds of food simulation solutions were prepared. After the test of soaking, the solutions were detected by UPLC-MS/MS.Oleamide was separated by ZORBAX C_18(3.0 mm×100 mm, 1.8 μm) hromatographic column. The eluent was qualitatively and quantitatively determined by mass spectrometer with electrospray ionization in positive multiple reaction monitoring mode. Results Oleamide had good linear relationship in 5 kinds of food simulation solutions in the range of 0.25-5.0 mg/L with correlation coefficients more than 0.9990. The limits of detection of oleamide were 0.001-0.002 mg/L, the limit of quantification was 0.003-0.005 mg/L. The recoveries of oleamide at 3 spiked levels were 90.3%-117.1%, and the relative standard deviations(RSDs) were 0.20%-2.10%(n=6). Conclusion This method is accurate and reliable, which is suitable for the determination of oleamide migration in 5 kinds of food simulation solutions.
Objective To establish a method for the determination of oleamide migration from food contact materials by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods According to the GB5009.156-2016 National food safety standards-Food contact materials and products migration test pretreatment methods, 5 kinds of food simulation solutions were prepared. After the test of soaking, the solutions were detected by UPLC-MS/MS.Oleamide was separated by ZORBAX C_18(3.0 mm×100 mm, 1.8 μm) hromatographic column. The eluent was qualitatively and quantitatively determined by mass spectrometer with electrospray ionization in positive multiple reaction monitoring mode. Results Oleamide had good linear relationship in 5 kinds of food simulation solutions in the range of 0.25-5.0 mg/L with correlation coefficients more than 0.9990. The limits of detection of oleamide were 0.001-0.002 mg/L, the limit of quantification was 0.003-0.005 mg/L. The recoveries of oleamide at 3 spiked levels were 90.3%-117.1%, and the relative standard deviations(RSDs) were 0.20%-2.10%(n=6). Conclusion This method is accurate and reliable, which is suitable for the determination of oleamide migration in 5 kinds of food simulation solutions.
引文
[1]陈志峰.塑料食品包装材料中有毒有害化学残留物及分析方法[J].食品与机械,2006,22(2):3-7.Chen ZF.Test and analysis methods for chemical contaminants in plastic food packing materials[J].Food Mach,2006,22(2):3-7.
[2]GB 9685-2016食品安全国家标准食品接触材料及制品用添加剂使用标准[S].GB 9685-2016 National food safety standard-Uses of additives in food contact materials and their products[S].
[3]吴贵岚.油酸酰胺在塑料中的应用[J].塑料助剂,2000,1(19):22-24.Wu GL.Application of oleic acid amide in plastics[J].Plast Addit,2000,1(19):22-24.
[4]郭长彬,宋宏锐.内源性睡眠诱导物质油酸胺的研究迚展[J].中国药物化学杂志,2000,10(4):300-304.Guo CB,Song HR.The development of oleamide-an endogenous sleep-inducing lipid[J].Chin J Med Chem,2000,10(4):300-304.
[5]Arafat ES,Trimble JW,Andersen RN,et al.Identification of fatty acid amides in human plasma[J].Lif Sci,1989,45:1679-1687.
[6]Lin G,Zhu MM,Yang JY,et al.Differential proteomic analysis of the anti-depressive effects of oleamide in a rat chronic mild stress model of depression[J].Pharmacol Biochem Behav,2015,(131):77-86.
[7]Fu J,Astarita G,Gaetani S,et al.Food intake regulates oleoylethanolanmind formation and degradation in the proximal small intestine[J].J Biol Chem,2007,282(2):1518-1528.
[8]Robinhiley C,Hoi PM.Oleamide:A Fatty acid amide signaling molecule in the cardiovascular system[J].Cardiovasc Drug Rev,2007,25(1):46-60.
[9]蔡翔宇,江思华,吴玉杰,等.超高效液相色谱-串联质谱法同时检测功能食品中6种玛咖酰胺[J].食品安全质量检测学报,2018,9(7):1628-1633.Cai XY,Jiang SH,Wu YJ,et al.Simultaneous determination of 6 kinds of Maca amids in functional foods by ultra performance liquid chromatography-tandem mass spectrometry[J].J Food Saf Qual,2018,9(7):1628-1633.
[10]朱财延,李炳辉,罗成员,等.高效液相色谱-质谱法分析植物玛咖中的玛咖烯和玛咖酰胺[J].分析仪器,2014,(5):44-49.Zhu CY,Li BH,Luo CY,et al.Analysis of macaenes and macamides in maca plant by high performance liquid chromatography-mass spectrometry[J].Anal Instrum,2014,(5):44-49.
[11]夏陈,邓俊林,张盈娇,等.高效液相色谱测定川产玛咖中N-苄基-十六烷酰胺的含量[J].化学与生物工程,2017,34(2):68-70.Xia C,Deng JL,Zhang YJ,et al.Determination of contents of N-benzyl-hexadecanaminde in Sichuan maca by HPLC[J].Chem Bioeng,2017,34(2):68-70.
[12]吴春英,白鹭,谷风,等.固相萃取-超高效液相色谱-串联质谱法同时测定地表水中的18种酰胺类除草剂[J].理化检测-化学分册,2016,52(5):602-606.Wu CY,Bai L,Gu F,et al.Simultaneous determination of 18 amide herbicides in surface water by SPE-UPLC-MS/MS[J].Ptca Part B Chem Anal,2016,52(5):602-606.
[13]高大方,张泽生.新资源食品玛咖中功能成分的UPLC-MS/MS研究[J].安徽农业科学,2013,41(2):830-832.Gao DF,Zhang ZS.Functional constituents identification in maca,a novel food by UPLC-MS/MS[J].J Anhui Agric Sci,2013,41(2):830-832.
[14]杨军,王艳菊,白永文,等.关于同时检测五种不同玛咖酰胺含量方法的探讨[J].农业与技术,2018,38(8):25-26.Yang J,Wang YJ,Bai YW,et al.Discussion on the method of simultaneous detection of 5 different maca amide content[J].Agric Technol,2018,38(8):25-26.
[15]陈蔷,宋志超,张崇威,等.动物源食品中酰胺醇类药物及其代谢物残留检测超高效液相色谱-串联质谱法研究[J].中国兽药杂志,2015,49(8):28-34.Chen Q,Song ZQ,Zhang CW,et al.Determination of amphenicols and metabolite residues in animal derived food by UPLC-MS/MS[J].Chin JVet,2015,49(8):28-34.
[16]王兴宁.气相色谱-串联质谱检测烟草中10种酰胺类除草剂残留[J].贵州师范大学学报(自然科学版),2017,35(5):85-89.Wang XN.Determination of 10 kinds of acetanilide herbicide in tobacco by gas chromatography-tandem mass spectrometry[J].J Guizhou Norm Univ(Nat Sci Ed),2017,35(5):85-89.
[17]方宁,王子剑,赵劲松,等.气相色谱-质谱法测定食品接触材料润滑剂在脂类食品模拟物中迁移量[J].中国食品卫生杂志,2016,28(3):319-322.Fang N,Wang ZJ,Zhao JS,et al.Determination of lubricant migration from food contact materials to the lipid food stimulant by chromatography-mass spectrometry[J].Chin J Food Hyg,2016,28(3):319-322
[18]方宁,巩俐彤,李倩,等.气相色谱-质谱法测定食品接触材料中4种润滑剂的迁移量[J].中国食品卫生杂志,2014,26(6):562-565.Fang N,Gong LT,Li Q,et al.Determination of 4 kinds of migration of lubricant in food contact materials by gas chromatography-mass spectrometry[J].Chin J Food Hyg,2014,26(6):562-565.
[19]Lv G,Wang LB,Liu J,et al.Method for determination of fatty acid amides in polyethylene packaging materials-Gas chromatography/mass spectrometry[J].J Chromatogr A,2009,(1216):8545-8548.
[20]GB 5009.156-2016食品安全国家标准食品接触材料及制品迁移试验预处理方法通则[S].GB 5009.156 National food safety standards-Food contact materials and products migration test pretreatment methods[S].
[2]GB 9685-2016食品安全国家标准食品接触材料及制品用添加剂使用标准[S].GB 9685-2016 National food safety standard-Uses of additives in food contact materials and their products[S].
[3]吴贵岚.油酸酰胺在塑料中的应用[J].塑料助剂,2000,1(19):22-24.Wu GL.Application of oleic acid amide in plastics[J].Plast Addit,2000,1(19):22-24.
[4]郭长彬,宋宏锐.内源性睡眠诱导物质油酸胺的研究迚展[J].中国药物化学杂志,2000,10(4):300-304.Guo CB,Song HR.The development of oleamide-an endogenous sleep-inducing lipid[J].Chin J Med Chem,2000,10(4):300-304.
[5]Arafat ES,Trimble JW,Andersen RN,et al.Identification of fatty acid amides in human plasma[J].Lif Sci,1989,45:1679-1687.
[6]Lin G,Zhu MM,Yang JY,et al.Differential proteomic analysis of the anti-depressive effects of oleamide in a rat chronic mild stress model of depression[J].Pharmacol Biochem Behav,2015,(131):77-86.
[7]Fu J,Astarita G,Gaetani S,et al.Food intake regulates oleoylethanolanmind formation and degradation in the proximal small intestine[J].J Biol Chem,2007,282(2):1518-1528.
[8]Robinhiley C,Hoi PM.Oleamide:A Fatty acid amide signaling molecule in the cardiovascular system[J].Cardiovasc Drug Rev,2007,25(1):46-60.
[9]蔡翔宇,江思华,吴玉杰,等.超高效液相色谱-串联质谱法同时检测功能食品中6种玛咖酰胺[J].食品安全质量检测学报,2018,9(7):1628-1633.Cai XY,Jiang SH,Wu YJ,et al.Simultaneous determination of 6 kinds of Maca amids in functional foods by ultra performance liquid chromatography-tandem mass spectrometry[J].J Food Saf Qual,2018,9(7):1628-1633.
[10]朱财延,李炳辉,罗成员,等.高效液相色谱-质谱法分析植物玛咖中的玛咖烯和玛咖酰胺[J].分析仪器,2014,(5):44-49.Zhu CY,Li BH,Luo CY,et al.Analysis of macaenes and macamides in maca plant by high performance liquid chromatography-mass spectrometry[J].Anal Instrum,2014,(5):44-49.
[11]夏陈,邓俊林,张盈娇,等.高效液相色谱测定川产玛咖中N-苄基-十六烷酰胺的含量[J].化学与生物工程,2017,34(2):68-70.Xia C,Deng JL,Zhang YJ,et al.Determination of contents of N-benzyl-hexadecanaminde in Sichuan maca by HPLC[J].Chem Bioeng,2017,34(2):68-70.
[12]吴春英,白鹭,谷风,等.固相萃取-超高效液相色谱-串联质谱法同时测定地表水中的18种酰胺类除草剂[J].理化检测-化学分册,2016,52(5):602-606.Wu CY,Bai L,Gu F,et al.Simultaneous determination of 18 amide herbicides in surface water by SPE-UPLC-MS/MS[J].Ptca Part B Chem Anal,2016,52(5):602-606.
[13]高大方,张泽生.新资源食品玛咖中功能成分的UPLC-MS/MS研究[J].安徽农业科学,2013,41(2):830-832.Gao DF,Zhang ZS.Functional constituents identification in maca,a novel food by UPLC-MS/MS[J].J Anhui Agric Sci,2013,41(2):830-832.
[14]杨军,王艳菊,白永文,等.关于同时检测五种不同玛咖酰胺含量方法的探讨[J].农业与技术,2018,38(8):25-26.Yang J,Wang YJ,Bai YW,et al.Discussion on the method of simultaneous detection of 5 different maca amide content[J].Agric Technol,2018,38(8):25-26.
[15]陈蔷,宋志超,张崇威,等.动物源食品中酰胺醇类药物及其代谢物残留检测超高效液相色谱-串联质谱法研究[J].中国兽药杂志,2015,49(8):28-34.Chen Q,Song ZQ,Zhang CW,et al.Determination of amphenicols and metabolite residues in animal derived food by UPLC-MS/MS[J].Chin JVet,2015,49(8):28-34.
[16]王兴宁.气相色谱-串联质谱检测烟草中10种酰胺类除草剂残留[J].贵州师范大学学报(自然科学版),2017,35(5):85-89.Wang XN.Determination of 10 kinds of acetanilide herbicide in tobacco by gas chromatography-tandem mass spectrometry[J].J Guizhou Norm Univ(Nat Sci Ed),2017,35(5):85-89.
[17]方宁,王子剑,赵劲松,等.气相色谱-质谱法测定食品接触材料润滑剂在脂类食品模拟物中迁移量[J].中国食品卫生杂志,2016,28(3):319-322.Fang N,Wang ZJ,Zhao JS,et al.Determination of lubricant migration from food contact materials to the lipid food stimulant by chromatography-mass spectrometry[J].Chin J Food Hyg,2016,28(3):319-322
[18]方宁,巩俐彤,李倩,等.气相色谱-质谱法测定食品接触材料中4种润滑剂的迁移量[J].中国食品卫生杂志,2014,26(6):562-565.Fang N,Gong LT,Li Q,et al.Determination of 4 kinds of migration of lubricant in food contact materials by gas chromatography-mass spectrometry[J].Chin J Food Hyg,2014,26(6):562-565.
[19]Lv G,Wang LB,Liu J,et al.Method for determination of fatty acid amides in polyethylene packaging materials-Gas chromatography/mass spectrometry[J].J Chromatogr A,2009,(1216):8545-8548.
[20]GB 5009.156-2016食品安全国家标准食品接触材料及制品迁移试验预处理方法通则[S].GB 5009.156 National food safety standards-Food contact materials and products migration test pretreatment methods[S].