亲水作用高效液相色谱-串联质谱法测定薯片及饼干中丙烯酰胺的含量
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摘要
目的建立亲水作用高效液相色谱-串联质谱法测定薯片及饼干中丙烯酰胺含量的分析方法。方法薯片及饼干经超纯水提取,正己烷除脂,Cleanert~?ACA固相萃取柱净化,BEH Amide色谱柱(2.1mm×100mm,1.7μm)分离,并以0.1%(V:V)甲酸水-乙腈溶液=2:8(V:V)为流动相,电喷雾正离子模式电离,多反应监测模式检测,内标法定量。结果丙烯酰胺在5～2000μg/L范围内线性关系良好,相关系数大于0.999。方法的检出限(S/N>3)和定量限(S/N>10)分别为3μg/kg和10μg/kg。在不同基质中,丙烯酰胺在20、200、1000μg/kg的添加水平下平均加标回收率为91.5%～98.2%,相对标准偏差为2.71%～4.82%。结论此方法具有准确度好、灵敏度高等特点,适用于薯片及饼干中丙烯酰胺的测定。
Objective To establish a method for determination of acrylamide in potato chips and biscuits by hydrophilic interaction-high performance liquid chromatography-tandem mass spectrometry. Methods Acrylamide in potato chips and biscuits was extracted with ultrapure water and purified with hexane and Cleanert~? ACA solid phase extraction. The separation was performed on BEH Amide chromatographic column(2.1 mm×100 mm, 1.7 μm)with the mobile phase of 0.1% formic acid solution-acetonitrile(2:8, V:V). It was monitored by positive electrospray ionization(ESI+) and multi reaction mode, and quantified by internal standard method. Results Acrylamide had good linear relationship in the range of 5-2000 g/L, and the correlation coefficients were greater than 0.999. The limit of detection(S/N>3) and limit of quantitative(S/N>10) were 3 μg/kg and 10 μg/kg, respectively. In different substrates, the recoveries at 3 spiked levels(20, 200 and 1000 μg/kg) were 91.5%-98.2%, with the relative standard deviations of 2.71%-4.82%. Conclusion This method is accurate and sensitive, which is suitable for determination of acrylamide in potato chips and biscuits.
Objective To establish a method for determination of acrylamide in potato chips and biscuits by hydrophilic interaction-high performance liquid chromatography-tandem mass spectrometry. Methods Acrylamide in potato chips and biscuits was extracted with ultrapure water and purified with hexane and Cleanert~? ACA solid phase extraction. The separation was performed on BEH Amide chromatographic column(2.1 mm×100 mm, 1.7 μm)with the mobile phase of 0.1% formic acid solution-acetonitrile(2:8, V:V). It was monitored by positive electrospray ionization(ESI+) and multi reaction mode, and quantified by internal standard method. Results Acrylamide had good linear relationship in the range of 5-2000 g/L, and the correlation coefficients were greater than 0.999. The limit of detection(S/N>3) and limit of quantitative(S/N>10) were 3 μg/kg and 10 μg/kg, respectively. In different substrates, the recoveries at 3 spiked levels(20, 200 and 1000 μg/kg) were 91.5%-98.2%, with the relative standard deviations of 2.71%-4.82%. Conclusion This method is accurate and sensitive, which is suitable for determination of acrylamide in potato chips and biscuits.
引文
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[11]程劼,苏晓鸥,张维,等.气相色谱-串联四极杆质谱测定餐厨废弃物中的丙烯酰胺[J].中国农业科学,2012,45(16):3373-3381.Cheng J,Su XO,Zhang W,et al.Determination of acrylamide in kitchen waste using gas chromatography-tandem mass spectrometry[J].Sci Agric Sin,2012,45(16):3373-3381.
[12]李吉平,刘文森,高宏伟,等.固相萃取HPLC联用法测定食品中丙烯酰胺含量的研究[J].食品科学,2007,28(2):250-254.Li JP,Liu WS,Gao HW,et al.Determination of food acrylamide with solid phase extraction and high performance liquid chromatography[J].Food Sci,2007,28(2):250-254.
[13]程江华,王薇,廖华俊,等.LC-MS/MS法测定11种鲜切油炸马铃薯片中丙烯酰胺的含量[J].中国食品学报,2011,7(11):176-179.Cheng JH,Wang W,Liao HJ,et al.Determination of acrylamide in 11fresh Fried potato slices by LC-MS/MS method[J].J Chin Inst Food Sci Technol,2011,7(11):176-179.
[14]阴永泼,卞华伟,李冰,等.QuEChERS前处理结合HPLC-MS法检测淀粉类食品中丙烯酰胺[J].食品科技,2017,42(5):284-289.Yin YP,Bian HW,Li B,et al.Determination of acrylamide in starchy foods by high performance liquid chromatography mass spectrometry combined with QuEChERS pretreatment[J].Food Sci Technol,2017,42(5):284-289.
[15]王浩,刘艳琴,杨红梅,等.高效液相色谱-串联四极杆质谱联用测定饼干中丙烯酰胺残留量[J].食品研究与开发,2009,30(2):108-110.Wang H,Liu YQ,Yang HM,et al.Determination of acrylamide in biscuit by chromatography-tandem quadrupole mass spectrometry[J].Food Res Dev,2009,30(2):108-110.
[16]虞成华,周泽琳,陆志芸,等.液质联用法测定米粉中三聚氰胺和丙烯酰胺[J].食品工业,2013,34(7):209-211.Yu CH,Zhou ZL,Lu ZY,et al.Determination of melamine and acrylamide in infant rice flour by liquid chromatography tandem mass spectrometry[J].Food Ind,2013,34(7):209-211.
[17]叶艳芬,徐立恒.固相萃取-高效液相色谱法测定面粉类食品中丙烯酰胺[J].分析试验室,2013,32(7):95-97.Ye YF,Xu LH.Determination of acrylamide in wheaten foods by solid-phase extraction and HPLC[J].Chin J Anal Lab,2013,32(7):95-97.
[2]廉保全,张方体,胡沛,等.丙烯酰胺职业危害调查[J].华北煤炭医学院学报,2000,2(5):502-503.Lian BQ,Zhang FT,Hu P,et al.Investigation of occupational hazard of acrylamide[J].J North China Coal Med Coll,2000,2(5):502-503.
[3]Wang H,Huang P,Lie TT,et al.Reproductive toxicity of acrylamide-treated male rats[J].Reprod Toxicol,2010,29(2):225-230.
[4]Ma YX,Shi J,Zheng MG,et al.Toxicological effects of acrylamide on the reproductive system of weaning male Rats[J].Toxicol Ind Health,2011,27(7):617-627.
[5]李百祥,刘东敏.丙烯酰胺对小鼠免疫毒性机制的初探[J].毒理学杂志,2005,19(4):305-306.Li BX,Liu DM.Mechanism of acrylamide-induced immune toxicity in mice[J].J Toxicol,2005,19(4):305-306.
[6]Johnson KA,Gorzinski SJ,Bodner KM,et al.Chronic toxicity and oncogenicity study on acrylamide incorporated in the drinking water of fischer 344 rats[J].Toxicol Appl Pharm,1986,85(2):154-168.
[7]汪恩婷.丙烯酰胺及其代谢产物对小鼠所致氧化损伤和潜在致癌性的研究[D].长春:吉林大学,2015.Wang ET.Oxidative damage and potential carcinogenicity induced by acrylamide and its metabolite on mice[D].Changchun:Jilin University,2015.
[8]Zhang Y,Zhang Y.Formation and reduction of acrylamide in Maillard reaction:A review based on the current state of knowledge[J].Crit Rev Food Sci Nutr,2007,47(5):521-542.
[9]孙秀兰,纪剑,安璐,等.丙烯酰胺样品前处理及其检测方法研究进展[J].食品与生物技术学报,2013,32(5):456-459.Sun XL,Ji J,An L,et al.Acrylamide sample preparation and detection method research progress[J].J Food Sci Biotechnol,2013,32(5):456-459.
[10]Vikstrom AC,Abramsson-Zetterberg L,Naruszewicz M,et al.In vivo doses of acrylamide and glycidamide in humans after intake of acrylamide-rich food[J].Toxicol Sci,2011,119(1):41-49.
[11]程劼,苏晓鸥,张维,等.气相色谱-串联四极杆质谱测定餐厨废弃物中的丙烯酰胺[J].中国农业科学,2012,45(16):3373-3381.Cheng J,Su XO,Zhang W,et al.Determination of acrylamide in kitchen waste using gas chromatography-tandem mass spectrometry[J].Sci Agric Sin,2012,45(16):3373-3381.
[12]李吉平,刘文森,高宏伟,等.固相萃取HPLC联用法测定食品中丙烯酰胺含量的研究[J].食品科学,2007,28(2):250-254.Li JP,Liu WS,Gao HW,et al.Determination of food acrylamide with solid phase extraction and high performance liquid chromatography[J].Food Sci,2007,28(2):250-254.
[13]程江华,王薇,廖华俊,等.LC-MS/MS法测定11种鲜切油炸马铃薯片中丙烯酰胺的含量[J].中国食品学报,2011,7(11):176-179.Cheng JH,Wang W,Liao HJ,et al.Determination of acrylamide in 11fresh Fried potato slices by LC-MS/MS method[J].J Chin Inst Food Sci Technol,2011,7(11):176-179.
[14]阴永泼,卞华伟,李冰,等.QuEChERS前处理结合HPLC-MS法检测淀粉类食品中丙烯酰胺[J].食品科技,2017,42(5):284-289.Yin YP,Bian HW,Li B,et al.Determination of acrylamide in starchy foods by high performance liquid chromatography mass spectrometry combined with QuEChERS pretreatment[J].Food Sci Technol,2017,42(5):284-289.
[15]王浩,刘艳琴,杨红梅,等.高效液相色谱-串联四极杆质谱联用测定饼干中丙烯酰胺残留量[J].食品研究与开发,2009,30(2):108-110.Wang H,Liu YQ,Yang HM,et al.Determination of acrylamide in biscuit by chromatography-tandem quadrupole mass spectrometry[J].Food Res Dev,2009,30(2):108-110.
[16]虞成华,周泽琳,陆志芸,等.液质联用法测定米粉中三聚氰胺和丙烯酰胺[J].食品工业,2013,34(7):209-211.Yu CH,Zhou ZL,Lu ZY,et al.Determination of melamine and acrylamide in infant rice flour by liquid chromatography tandem mass spectrometry[J].Food Ind,2013,34(7):209-211.
[17]叶艳芬,徐立恒.固相萃取-高效液相色谱法测定面粉类食品中丙烯酰胺[J].分析试验室,2013,32(7):95-97.Ye YF,Xu LH.Determination of acrylamide in wheaten foods by solid-phase extraction and HPLC[J].Chin J Anal Lab,2013,32(7):95-97.