Determination of biogenic amines in aquatic products by modified Qu ECh ERS method and liquid chromatography-mass spectrometry
-
摘要: 采用改进的Qu ECh ERS方法,利用液相色谱-串联质谱(RPLC-TMS)检测,建立了几种水产品中生物胺的分析方法。样品用乙腈+甲醇(9+1)提取,无水硫酸钠除去水分,经乙二胺-N-丙基硅烷(PSA)和C18混合粉末净化,采用HILIC柱,以乙腈/1%甲酸水溶液为流动相梯度洗脱进行液相色谱分离。质谱分析采用电喷雾正离子电离,多反应监测模式,外标法定量。结果显示6种生物胺在10200 ng/m L范围线性关系良好。方法的定量限(LOQ,信噪比为10)为0.10 mg/kg。加标水平在0.10 mg/kg时,鱼、虾、蟹及鱿鱼四种阴性基质中加标的回收率在74.18%90.15%之间,相对标准偏差(RSD,n=6)在2.22%8.04%之间。结果表明本方法简便、快速、安全、适用于水产品中生物胺含量的定性和定量检测。
-
关键词:
- Qu ECh ERS /
- 液相色谱-串联质谱 /
- 生物胺 /
- 水产品 /
- 检测
Abstract: A modified Qu ECh ERS method followed by liquid chromatography- tandem mass spectrometric analysis was developed for the determination of biogenic amines in aquatic products. The samples was diluted with acetonitrile / methanol solution( 9 /1) and cleaned up with primary secondary amine( PSA) and Octadecylsilane( C18) sorbent.The separation of biogenic amines was performed by hydrophilic interaction liquid chromatography( HILIC) column and gradiently eluting with acetonitrile/formic acid- water( 1%) without derivatization. Biogenic amines were analyzed by positive electrosprary ionization( ESI~+) tandem mass spectrometry under multiple reaction monitoring( MRM) mode.Quantification was achieved using external standard method.The linearities were excellent in the range of 10~200 ng / m L.The limits of quantification( LOQ,S / N = 10) were 0.10 mg / kg.The recoveries of biogenic amines spiked in matrices were between 74.18% and 90.15% at the spiked levels of 0.10 mg / kg. The relative standard deviations( RSDs,n = 6) were in the range of 2.22% ~8.04%.The method( quick,easy,safe) could meet the requirements of the daily work for the determination of biogenic amines in aquatic products.-
Keywords:
- QuEChERS /
- RPLC-TMS /
- biogenic amines /
- aquatic products /
- determination
-
[1] Silla Santos M H.Biogenic amines:Their importance in foods.[J].International Journal of Food Microbiology,1996,29:213-231.
[2] Shalaby A R.Significance of biogenic amines to food safety and human health.[J].Food Research International,1996,29:675-690.
[3] 赵中辉.水产品贮藏中生物胺的变化及组胺形成机制研究[D].青岛:中国海洋大学,2011. [4] Anastassiades M,Lehotay S J,Stajnbaher D,et al.Fast and easy multiresidue method employing acetonitrile extraction/partitioning and“dispersive solid-phase extraction”for the determination of pesticide residues in produce.[J].J AOAC Int,2003,86(2):412-431.
[5] 刘亚伟,董一威,孙宝利,等.Qu ECh ERS在食品中农药多残留检测的应用研究进展[J].食品科学,2009,30(9):285-289. [6] Armagan Onal.A review:Current analytical methods for the determination of biogenic amines in foods[J].Food Chemistry,2007,103:1475-1486.
[7] 崔晓美,陈树兵,陈杰,等.基质分散固相萃取-亲水作用色谱-串联质谱法测定鲣鱼中5种生物胺的含量[J].分析化学,2013,41(12):1869-1874. [8] 孙亚军,廖建萌,雷晓凌,等.液相色谱-串联质谱法同时测定虾仁中八种生物胺[J].食品工业,2015,36(3):273-277. [9] Calbiani F,Careri M,Elviri L,et al.Rapid assay for analyzing biogenic amines in cheese:matrix solid-phase dispersion followed by liquid chromatography-electrospray-tandem mass spectrometry[J].J Agric Food Chem,2005,53:3779-3783.
[10] Klinsunthorn N,Petsom A,Nhujak T.Determination of steroids adulterated in liquid herbal medicines using Qu ECh ERS sample preparation and high-performance liquid chromatography[J].J Pharm Biom Anal,2011,55(5):1175-1178.
[11] 丁涛,吕辰,柳菡,等.高效液相色谱-四级杆/静电场轨道阱高分辨质谱检测葡萄酒中8中生物胺[J].分析测试学报,2014,33(1):27-33. [12] 周杨,冯群科,朱永林.高效液相色谱-串联质谱法测定饲料中三聚氰胺[J].中国饲料,2010(12):33-36. [13] 吴云辉,周爽,徐敦明.非衍生化液相色谱-串联质谱法测定动物源性食品中8种生物胺[J].色谱,2013,31(2):111-116.
计量
- 文章访问数:
- HTML全文浏览量:
- PDF下载量: