Scott P M, Lawrence G A
Health and Welfare Canada, Bureau of Chemical Safety, Food Research Division, Ottawa, Ontario.
J Assoc Off Anal Chem. 1988 Nov-Dec;71(6):1176-9.
Previous research has demonstrated transmission of zearalenone and alpha- and beta-zearalenols into the milk of cows and other animals. Since human intake of zearalenone and its metabolites via milk is an unknown factor in risk assessment of zearalenone and because appropriate methodology for their determination in milk is not available, a rapid and sensitive analytical method has been developed. Essentially, the method includes extraction with basic acetonitrile, acidification, partition into methylene chloride on a hydrophilic matrix, cleanup on an aminopropyl solid phase extraction column, and reverse-phase liquid chromatography with fluorescence detection. Recoveries from milk averaged 84% for zearalenone, 93% for alpha-zearalenol, and 90% for beta-zearalenol at spiking levels of 0.5 to 20 ng/mL. As little as 0.2 ng/mL of zearalenone and alpha-zearalenol and 2 ng/mL of beta-zearalenol can be detected in milk. These 3 compounds are stable in refrigerated milk for at least 2 weeks and in milk brought to boiling. Enzymes (beta-glucuronidase and aryl sulfatase) may be added to milk prior to extraction to hydrolyze any conjugates.
先前的研究已证明玉米赤霉烯酮以及α-和β-玉米赤霉醇可转移至奶牛和其他动物的乳汁中。由于人类通过牛奶摄入玉米赤霉烯酮及其代谢物在玉米赤霉烯酮风险评估中是一个未知因素，且目前尚无测定牛奶中这些物质的合适方法，因此开发了一种快速灵敏的分析方法。该方法主要包括用碱性乙腈萃取、酸化、在亲水性基质上分配至二氯甲烷、在氨丙基固相萃取柱上净化以及采用荧光检测的反相液相色谱法。在0.5至20 ng/mL的加标水平下，牛奶中玉米赤霉烯酮的平均回收率为84%，α-玉米赤霉醇为93%，β-玉米赤霉醇为90%。牛奶中可检测到低至0.2 ng/mL的玉米赤霉烯酮和α-玉米赤霉醇以及2 ng/mL的β-玉米赤霉醇。这3种化合物在冷藏牛奶中至少可稳定保存2周，在煮沸的牛奶中也稳定。在萃取前可向牛奶中添加酶（β-葡萄糖醛酸酶和芳基硫酸酯酶）以水解任何共轭物。
