Beljaars P R, Schumans J C, Koken P J
J Assoc Off Anal Chem. 1975 Mar;58(2):263-71.
A study is presented for the quantitative fluorodensitometric analysis of aflatoxins in spices, in particular nutmeg (Semen myristicae). Samples were extracted with chloroform, followed by silica gel column cleanup according to the AOAC officail first action method, 26.019(a), and by 2-dimensional thin layer chromatography according to the antidiagonal technique. The method includes a confirmatory test for aflatoxins by hemiacetal formation. The concentrations of aflatoxins in samples were determined by measurement of the fluorescent intensities of the separated aflatoxin spots from sample and standards on the same chromato-plate with a reflectance flying-spot sensitometer. With such a technique, a coefficient of variation value of 5.22 plus or minus 1.24% (P = 99%) was calculated for a series of 5 standard B-1 spots and averaged for 13 TLC plates, demonstrating the precision of the chromatographic and densitometric procedures. An average recovery of 108.4 plus or minus 5.8% (P = 95%) was obtained for 11 spiked nutmeg extracts (5.0-20.0 mu-g B-1 added/kg), whereas an average recovery of 92.6 plus or minus 4.9 (P = 95%) was established for 13 spiked nutmeg samples (5.0-20.0 mu-g B-1 added/kg). The coefficient of variation of the complete analytical procedure for ground nutmeg was 8.80%. In a survey on the occurrence of aflatoxins in 40 commercial nutmeg samples (covering 12 different brands) in The Netherlands, aflatoxins were detected in 30 ground samples (32 ground samples analyzed) in concentrations ranging from 1.0 to 23.2 mu-g B-1/kg or 2.7 to 36.5 mu-g B-1 + B-2 + G-1 + G-2/kg, whereas no aflatoxins were present in whole nutmeg kernels (8 samples analyzed). The lowest level of detection was 1.0 mu-g B-1/kg. In addition, 50 commercial spices consisting of 19 different types of commodities other than nutmeg wer assayed for aflatoxins according to the same procedure. No aflatoxins were detected in these samples, with the exception of 1 sample of bay leaf which contained 5.1 mu-g B-1/kg.
本文介绍了一种用于定量分析香料特别是肉豆蔻（肉豆蔻种子）中黄曲霉毒素的荧光光密度分析法。样品用氯仿提取，然后按照美国官方分析化学家协会（AOAC）的首次行动方法26.019(a)进行硅胶柱净化，并按照对角线技术进行二维薄层色谱分析。该方法包括通过半缩醛形成对黄曲霉毒素进行确证试验。通过用反射飞点光度计测量同一色谱板上样品和标准品中分离出的黄曲霉毒素斑点的荧光强度，来测定样品中黄曲霉毒素的浓度。采用这种技术，对一系列5个标准B-1斑点进行计算，在13块薄层色谱板上平均得到变异系数值为5.22±1.24%（P = 99%），证明了色谱和光密度分析程序的精密度。对于11个加标肉豆蔻提取物（添加量为5.0 - 20.0μg B-1/kg），平均回收率为108.4±5.8%（P = 95%）；而对于13个加标肉豆蔻样品（添加量为5.0 - 20.0μg B-1/kg），平均回收率为92.6±4.9（P = 95%）。磨碎肉豆蔻完整分析程序的变异系数为8.80%。在对荷兰40个商业肉豆蔻样品（涵盖12个不同品牌）中黄曲霉毒素存在情况的调查中，在30个磨碎样品（共分析32个磨碎样品）中检测到黄曲霉毒素，浓度范围为1.0至23.2μg B-1/kg或2.7至36.5μg B-1 + B-2 + G-1 + G-2/kg，而在整个肉豆蔻仁（共分析8个样品）中未检测到黄曲霉毒素。最低检测水平为1.0μg B-1/kg。此外，按照相同程序对除肉豆蔻外的由19种不同商品组成的50种商业香料进行了黄曲霉毒素检测。除了1个含有5.1μg B-1/kg的月桂叶样品外，这些样品中均未检测到黄曲霉毒素。
