同位素稀释超高效液相色谱-串联质谱法测定中式炒菜中丙烯酰胺的含量
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摘要
目的建立中式炒菜中丙烯酰胺的同位素稀释超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。方法试样经正己烷除脂后加入丙烯酰胺同位素内标,以水提取,Carrez试剂和混合型强阳离子交换固相萃取柱净化,采用超高效液相色谱-串联质谱检测,内标法定量。结果丙烯酰胺在5μg/L～400μg/L浓度范围内线性良好,相关系数为0. 999 8。方法检出限为2μg/kg,定量限为6μg/kg。三个添加水平(10μg/kg、50μg/kg、100μg/kg)的回收率为81. 8%～117. 0%,相对标准偏差均小于10%。结论本方法准确、稳定,操作简捷,适用于中式炒菜中丙烯酰胺含量的测定。
Objective To establish a method for the determination of acrylamide in stir-fried dishes by ultra performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS). Methods The sample was spiked with acrylamide isotope internal standard after degreased with n-hexane. Acrylamide was extracted with water,and then cleaned up by Carrez reagent and strong cation-exchange( MCX) solid-phase extraction( SPE) cartridge. Acrylamide was analyzed by UPLC-MS/MS. The isotope was used as an internal standard for quantification. Results The calibration curve showed good linearity in the range of 5 μg/L-400 μg/L with a correlation coefficient of 0. 999 8. The limits of detection and quantification were 2 μg/kg and 6 μg/kg,respectively. The recoveries at three levels( 10 μg/kg,50 μg/kg and 100 μg/kg) ranged from 81. 8%-117. 0%with relative standard deviation less than 10%. Conclusion The method is suitable to determine acrylamide content in Chinese stir-fried dishes with the advantages of simplicity,high accuracy and good stability.
Objective To establish a method for the determination of acrylamide in stir-fried dishes by ultra performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS). Methods The sample was spiked with acrylamide isotope internal standard after degreased with n-hexane. Acrylamide was extracted with water,and then cleaned up by Carrez reagent and strong cation-exchange( MCX) solid-phase extraction( SPE) cartridge. Acrylamide was analyzed by UPLC-MS/MS. The isotope was used as an internal standard for quantification. Results The calibration curve showed good linearity in the range of 5 μg/L-400 μg/L with a correlation coefficient of 0. 999 8. The limits of detection and quantification were 2 μg/kg and 6 μg/kg,respectively. The recoveries at three levels( 10 μg/kg,50 μg/kg and 100 μg/kg) ranged from 81. 8%-117. 0%with relative standard deviation less than 10%. Conclusion The method is suitable to determine acrylamide content in Chinese stir-fried dishes with the advantages of simplicity,high accuracy and good stability.
引文
[1]王飞霞,张恒东,王雄权,等.丙烯酰胺作业人员职业健康检查结果分析[J].职业与健康,2016,32(22):3047-3049.
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[12]罗兰,任燕,柳洁.柱前衍生-气质联用法测定食品中的丙烯酰胺[J].现代预防医学,2016,43(7):1187-1190,1209.
[13]高志斌.高效液相色谱-串联质谱法测定各类食品中丙烯酰胺的实际应用[J].科技展望2016,26(33):94-95.
[14]中华人民共和国国家卫生和计划生育委员会.GB 5009.204-2014食品安全国家标准食品中丙烯酰胺的测定[S].北京:中国标准出版社,2015.
[2]毛丽君,赵金垣,徐希娴,等.急性丙烯酰胺中毒的临床特点[J].工业卫生与职业病,2017,43(1):58-60.
[3]Xu W,Sun JX,Bai S,et al.Effects of glycidamide on activity and progesterone biosynthesis of rat R2C Leydig cells[J].Agricultura Science&Technology,2015,36(6):1187-1190.
[4]Recio L,Friedman M,Marroni D,et al.Impact of acrylamide on Calcium signaling and cytoskeletal filaments in testes from F344 rat[J].International Journal of Toxicology,2017,36(2):124-132.
[5]Katen AL,Chambers CG,Nixon B,et al.Chronic acrylamide exposure in male mice results in elevated DNA damage in the germline and heritable induction of CYP2E1 in the testes[J].Biology of Reproduction,2016,95(4):1-15.
[6]Maronpot RR,Thoolen R,Hansen B.Two-year carcinogenicity study of acrylamide in Wistar Han rats with in utero exposure[J].Experimental and Toxicologic Pathology,2015,67(2):189-195.
[7]Collí-DuláRC,Friedman MA,Hansen B,et al.Transcriptomics analysis and hormonal changes of male and female neonatal rats treated chronically with a low dose of acrylamide in their drinking water[J].Toxicology Reports,2016,3:414-426.
[8]World Health Organization,International Agency for Research on Cancer.IARC monographs on the evaluation of carcinogenic risks to humans:Volume 60:Some industrial chemicals[M].Lyon:IARC,1994:389-433.
[9]Centre for Food Safety.The First Hong Kong Total Diet Study Report No.6:The First Hong Kong Total Diet Study:Acrylamide[EB/OL].[2018-12-22].http://www.cfs.gov.hk/english/programme/programme_firm/files/The_first_HKTDS_acrylamide_final_e.pdf.
[10]Gao J,Zhao YF,Zhu F,et al.Dietary exposure of acrylamide from the fifth Chinese Total Diet Study[J].Food and Chemica Toxicology,2016,87:97-102.
[11]Food and Agriculture Organization of the United Nations,World Health Organization.World technical report series:no.959:Evaluation of certain contaminants in food:Seventy-second repor of the joint FAO/WHO expert committee on food additives[M].Geneva:WHO,2011:9-21.
[12]罗兰,任燕,柳洁.柱前衍生-气质联用法测定食品中的丙烯酰胺[J].现代预防医学,2016,43(7):1187-1190,1209.
[13]高志斌.高效液相色谱-串联质谱法测定各类食品中丙烯酰胺的实际应用[J].科技展望2016,26(33):94-95.
[14]中华人民共和国国家卫生和计划生育委员会.GB 5009.204-2014食品安全国家标准食品中丙烯酰胺的测定[S].北京:中国标准出版社,2015.