Bacaloni Alessandro, Cavaliere Chiara, Cucci Francesca, Foglia Patrizia, Samperi Roberto, Laganà Aldo
Department of Chemistry, Sapienza University, Piazzale Aldo Moro 5, 00185 Rome, Italy.
J Chromatogr A. 2008 Feb 1;1179(2):182-9. doi: 10.1016/j.chroma.2007.11.081. Epub 2007 Dec 3.
A sensitive and reliable liquid chromatography-tandem mass spectrometric with electrospray ionization method for determining aflatoxins in hazelnuts has been developed. Three different extraction techniques, such as homogenization, ultrasonic extraction, and matrix solid phase dispersion have been tested and compared in terms of recovery, matrix effect, accuracy and precision. Ultrasound extraction was the most performing sample preparation method. Absolute recoveries for analytes and I.S. ranged from 93 to 101%. Accuracy and precision were calculated using matrix matched calibration, and ranged 91-102% and 2-11%, respectively. CC alpha and CC beta for aflatoxin B1 (EU limit=2 microg/kg) were 2.15 and 2.33 microg/kg, respectively. A ruggedness test performed on three other matrices demonstrated that sonication time was critical and a matrix matched calibration must be constructed for every sort of matrix.
已开发出一种灵敏且可靠的液相色谱-串联质谱结合电喷雾电离法，用于测定榛子中的黄曲霉毒素。测试并比较了三种不同的提取技术，即匀浆法、超声提取法和基质固相分散法，比较内容包括回收率、基质效应、准确度和精密度。超声提取是性能最佳的样品制备方法。分析物和内标的绝对回收率在93%至101%之间。使用基质匹配校准计算准确度和精密度，其范围分别为91-102%和2-11%。黄曲霉毒素B1的CCα和CCβ（欧盟限量=2微克/千克）分别为2.15和2.33微克/千克。对其他三种基质进行的耐用性测试表明，超声处理时间至关重要，并且必须针对每种基质构建基质匹配校准。
