Park D L, Diprossimo V, Abdel-Malek E, Trucksess M W, Nesheim S, Brumley W C, Sphon J A, Barry T L, Petzinger G
J Assoc Off Anal Chem. 1985 Jul-Aug;68(4):636-40.
An interlaboratory study of a negative ion chemical ionization mass spectrometric (MS) confirmation procedure for aflatoxin B1 was conducted in laboratories in the United States, England, and West Germany. Twelve partially purified, dry film extracts from naturally and artificially contaminated roasted peanuts, cottonseed, and ginger root containing varying quantities of aflatoxin B1 were distributed to the participating laboratories. The extracts required additional cleanup before MS analysis, using either an acidic alumina column and preparative thin layer chromatography (TLC) or a 2-dimensional TLC procedure. Recovery of purified aflatoxin B1 was influenced by the degree of recovery of sample from acid alumina and/or the TLC plate and incomplete elution of aflatoxin B1 from silica gel. Factors affecting MS confirmation included the purity and recovery of aflatoxin and MS instrument sensitivity. Aflatoxin B1 identity was confirmed in 19.5, 90.9, and 100% of samples containing less than 5, 5-10, and greater than 10 ng aflatoxin B1/g product, respectively, by solid probe introduction using full mass scans. The MS method has been adopted official first action.
美国、英国和西德的实验室开展了一项针对黄曲霉毒素B1的负离子化学电离质谱(MS)确证程序的实验室间研究。从天然和人工污染的烤花生、棉籽及姜根中提取了12份含有不同含量黄曲霉毒素B1的部分纯化干膜提取物,并分发给参与研究的实验室。在进行质谱分析之前,提取物需要使用酸性氧化铝柱和制备型薄层色谱法(TLC)或二维TLC程序进行额外净化。纯化黄曲霉毒素B1的回收率受样品从酸性氧化铝和/或TLC板上的回收程度以及黄曲霉毒素B1从硅胶上洗脱不完全的影响。影响质谱确证的因素包括黄曲霉毒素的纯度和回收率以及质谱仪的灵敏度。通过使用全质量扫描的固体探头进样,分别在含有低于5、5 - 10和高于10 ng黄曲霉毒素B1/克产品的样品中,有19.5%、90.9%和100%的样品确证了黄曲霉毒素B1的身份。该质谱方法已被采用为官方首次行动方法。