Zöllner P, Berner D, Jodlbauer J, Lindner W
Institute of Analytical Chemistry, University of Vienna, Austria.
J Chromatogr B Biomed Sci Appl. 2000 Feb 11;738(2):233-41. doi: 10.1016/s0378-4347(99)00521-6.
A fast, robust and sensitive LC-MS-MS method for the determination of zearalenone (ZON) and its metabolites alpha-zearalenol (alpha-ZOL) and beta-zearalenol (beta-ZOL) in beer samples is described. Sample preparation was performed by direct RP-18 solid-phase extraction of undiluted beer samples followed by selective determination of analytes by LC-MS-MS applying an atmospheric pressure chemical ionization (APCI) interface. Using the negative ion mode limits of determination of 0.03-0.06 microg l(-1) beer and limits of quantification of 0.07-0.15 microg l(-1) beer were achieved, which was distinctly more sensitive than in the positive ion mode. Twenty-three beer samples from different countries, produced from different grains and under different brewing conditions, were investigated by this method, but only in one sample could beta-ZOL and ZON be detected. Independently of the type of beer, relative standard deviations between 2.1% and 3.3%, a linear working range of 0.15 microg l(-1) to 500 microg l(-1) beer and recovery rates around 100% could be achieved when zearalanone (ZAN) was used as internal standard.
本文描述了一种快速、稳健且灵敏的液相色谱-串联质谱法,用于测定啤酒样品中的玉米赤霉烯酮(ZON)及其代谢物α-玉米赤霉醇(α-ZOL)和β-玉米赤霉醇(β-ZOL)。样品制备通过对未稀释的啤酒样品进行直接反相-18固相萃取,然后采用大气压化学电离(APCI)接口的液相色谱-串联质谱法对分析物进行选择性测定。在负离子模式下,啤酒的测定限为0.03 - 0.06 μg l⁻¹,定量限为0.07 - 0.15 μg l⁻¹,明显比正离子模式更灵敏。采用该方法对来自不同国家、由不同谷物在不同酿造条件下生产的23个啤酒样品进行了研究,但仅在一个样品中检测到了β-ZOL和ZON。无论啤酒类型如何,当使用玉米赤霉酮(ZAN)作为内标时,相对标准偏差在2.1%至3.3%之间,线性工作范围为0.15 μg l⁻¹至500 μg l⁻¹啤酒,回收率约为100%。