Development and validation of an analytical method for the analysis of Sterigmatocystin in roasted coffee beans and black pepper using liquid chromatography-tandem mass spectrometry

S. Chung, Andy H T Wu
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引用次数: 3

Abstract

ABSTRACT Sterigmatocystin (STC) is a toxic and potentially carcinogenic fungal toxin found in a variety of food commodities. This study describes the development of an analytical method to determine STC in roasted coffee beans and black pepper using ultra performance liquid chromatography (UPLC) coupled with triple quadrupole tandem mass spectrometry (MS/MS). 13C18-STC was used as internal standard. STC was extracted with a mixture of acetonitrile/water, diluted with a buffer, followed by purification with a solid-phase extraction and an immunoaffinity column prior to the UPLC-MS/MS analysis. Two multiple reaction monitoring (MRM) transitions were employed, one for quantification and one for confirmation of STC. The UPLC-MS/MS analytical method was validated with respect to selectivity, linearity, sensitivity, accuracy, precision, recovery, and stability. Calibration curves were linear over a concentration range 25–2,500 pg mL−1 with correlation coefficients (r) > 0.998. The method limit of quantification for STC in roasted coffee beans and black pepper was 0.10 μg kg−1. The accuracy and precision of the analytical method were acceptable within 15% at all quality control levels. This method was suitable to determine STC levels because of its selectivity, precision, and accuracy. The method was successfully applied to roasted coffee beans and black pepper samples. Graphical Abstract
液相色谱-串联质谱法分析烘焙咖啡豆和黑胡椒中sterigmatocytin的方法的建立与验证
Sterigmatocystin (STC)是一种存在于多种食品中的有毒和潜在致癌真菌毒素。建立了超高效液相色谱(UPLC) -三重四极杆串联质谱(MS/MS)测定烘焙咖啡豆和黑胡椒中STC的分析方法。13C18-STC作为内标。用乙腈/水的混合物提取STC,用缓冲液稀释,然后用固相萃取和免疫亲和柱纯化,然后进行UPLC-MS/MS分析。采用两次多反应监测(MRM)过渡,一次用于定量,一次用于STC的确认。对UPLC-MS/MS分析方法进行选择性、线性度、灵敏度、准确度、精密度、回收率和稳定性验证。在25 ~ 2500 pg mL−1的浓度范围内,校准曲线呈线性,相关系数(r)为> 0.998。焙烤咖啡豆和黑胡椒中STC的方法定量限为0.10 μ kg−1。在所有质量控制水平下,分析方法的准确度和精密度在15%以内是可接受的。该方法选择性好,精密度高,准确度高,适用于STC含量的测定。该方法成功地应用于烘焙咖啡豆和黑胡椒样品。图形抽象
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