Trucksess M W, Stack M E, Nesheim S, Page S W, Albert R H, Hansen T J, Donahue K F
Food and Drug Administration, Division of Contaminants Chemistry, Washington, DC 20204.
J Assoc Off Anal Chem. 1991 Jan-Feb;74(1):81-8.
An AOAC/IUPAC (International Union of Pure and Applied Chemistry) collaborative study was conducted to evaluate the effectiveness of an immunoaffinity column for the determination of aflatoxin. The test portion is extracted with methanol-water (7 + 3), filtered, diluted to less than 30% methanol with water, and applied to the affinity column. The column is washed with water and the concentrated aflatoxins are eluted with methanol. Total aflatoxins are determined by solution fluorometry with bromine (SFB), and individual toxins are determined by reverse-phase liquid chromatography with postcolumn derivatization with iodine (PCD). Corn naturally contaminated with aflatoxins, and peanuts, peanut butter, and corn containing added aflatoxins (B1:B2:G1:G2 = 7:1:3:1) were sent to 24 collaborators in the United States, France, Canada, and the Republic of South Africa. Twelve collaborators used the SFB method, 9 used the PCD method, and 3 used both SFB and PCD methods. Twenty collaborators completed the study (10 used the SFB method, 7 used the PCD method, and 3 used both SFB and PCD methods). Test portions were spiked at 10, 20, and 30 ng/g. For SFB analyses, recoveries of total aflatoxins were 123, 105, and 107%, respectively; the relative standard deviation for repeatability (RSDr) ranged from 11.75 to 16.57%, and the relative standard deviation for reproducibility (RSDR) ranged from 10.97 to 33.09%. For PCD analyses, recoveries were 81, 81, and 83%, respectively; the RSDr ranged from 5.20 to 17.22%, and the RSDR ranged from 4.68 to 50.77%. The RSDr for aflatoxins B1 and G1 for spiked test portions ranged from 5.45 to 23.55%, and the RSDR ranged from 4.21 to 57.28%.(ABSTRACT TRUNCATED AT 250 WORDS)
开展了一项美国官方分析化学师协会/国际纯粹与应用化学联合会（AOAC/IUPAC）合作研究，以评估免疫亲和柱用于测定黄曲霉毒素的有效性。将试验份用甲醇 - 水（7 + 3）萃取，过滤，用水稀释至甲醇含量低于30%，然后加至亲和柱上。用水冲洗柱子，并用甲醇洗脱浓缩的黄曲霉毒素。总黄曲霉毒素通过溴化溶液荧光法（SFB）测定，单个毒素通过柱后碘衍生化反相液相色谱法（PCD）测定。将天然受黄曲霉毒素污染的玉米以及添加了黄曲霉毒素（B1:B2:G1:G2 = 7:1:3:1）的花生、花生酱和玉米送交美国、法国、加拿大和南非共和国的24位协作人员。12位协作人员使用SFB方法，9位使用PCD方法，3位同时使用SFB和PCD方法。20位协作人员完成了研究（10位使用SFB方法，7位使用PCD方法，3位同时使用SFB和PCD方法）。试验份添加量为10、20和30 ng/g。对于SFB分析，总黄曲霉毒素的回收率分别为123%、105%和107%；重复性相对标准偏差（RSDr）为11.75%至16.57%，再现性相对标准偏差（RSDR）为10.97%至33.09%。对于PCD分析，回收率分别为81%、81%和83%；RSDr为5.20%至17.22%，RSDR为4.68%至50.77%。添加试验份中黄曲霉毒素B1和G1的RSDr为5.45%至23.55%，RSDR为4.21%至57.28%。（摘要截短于250字）
