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通过液相色谱-串联质谱法测定神经毒性剂作为小扁豆中普通野豌豆掺假的标志物。

Determination of neurotoxic agents as markers of common vetch adulteration in lentil by LC-MS/MS.

作者信息

Ghasemi Nesa, Secen Hasan, Yılmaz Hasibe, Binici Burcu, Goren Ahmet C

机构信息

Department of Chemistry, Faculty of Sciences, Ataturk University, 25240 Erzurum, Turkey.

TUBITAK UME (National Metrology Institute), Chemistry Group, Organic Chemistry Laboratories, P.O. Box 54, 41470 Gebze-Kocaeli, Turkey.

出版信息

Food Chem. 2017 Apr 15;221:2005-2009. doi: 10.1016/j.foodchem.2016.11.079. Epub 2016 Nov 24.

Abstract

Vicia sativa (common vetch), which contains β-cyanoalanine (BCA) and γ-glutamyl β-cyanoalanine (γGBCA) is used for adulteration of lentil and have neuro toxic effects on people and animals. Therefore the determination of BCA and γGBCA analytes in accurate and reliable manner has high importance for human and animal health. LC-IDMS/MS method has been developed and validated for quantitative analyses of β-cyanoalanine and C labeled BCA is used as an internal standard in γGBCA analysis. In order to validate the method, linearity, recovery, precision (repeatability), intermediate precision, limit of detection, and limit of quantification parameters were investigated. The correlation coefficient was found to be greater than 0.99 for both analytes. The recoveriess were determined as 95.8% for BCA and 97.4% for γGBCA. The relative expanded measurement uncertainties of β-cyanoalanine and γ-glutamyl-β-cyanoalanine were obtained as 4.6% and 5.8%, respectively with the coverage factor, k, is 2 and at 95% confidence level.

摘要

含有β-氰基丙氨酸(BCA)和γ-谷氨酰基β-氰基丙氨酸(γGBCA)的巢菜(普通野豌豆)被用于掺假小扁豆,并且对人和动物具有神经毒性作用。因此,以准确可靠的方式测定BCA和γGBCA分析物对人类和动物健康具有高度重要性。已开发并验证了LC-IDMS/MS方法用于β-氰基丙氨酸的定量分析,并且在γGBCA分析中使用C标记的BCA作为内标。为了验证该方法,研究了线性、回收率、精密度(重复性)、中间精密度、检测限和定量限参数。两种分析物的相关系数均大于0.99。BCA的回收率确定为95.8%,γGBCA的回收率确定为97.4%。在覆盖因子k为2且置信水平为95%时,β-氰基丙氨酸和γ-谷氨酰基-β-氰基丙氨酸的相对扩展测量不确定度分别为4.6%和5.8%。

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