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从大米中分离并通过液相色谱法测定环肽霉菌毒素环孢菌素A

Isolation and liquid chromatographic determination of the cyclic peptide mycotoxin cyclosporin A from rice.

作者信息

Edwards J V, Lillehoj E B

出版信息

J Assoc Off Anal Chem. 1987 Jan-Feb;70(1):126-9.

PMID:3558265
Abstract

A simple method for determination and quantitation of a cyclic peptide mycotoxin, cyclosporin A, in rice is presented. Rice inoculated with Trichoderma polysporum (Link ex Pers.) was extracted with methylene chloride after 4 weeks of incubation. Cyclosporin A was isolated from extracts by using open bed gel filtration column chromatography (LH-20, acetonitrile) and monitored with thin layer chromatography and reverse phase liquid chromatography coelution with a standard. Preliminary thin layer chromatographic methods were developed. Cyclosporin A was detected by iodine and after partial acid hydrolysis by ninhydrin and UV light. A liquid chromatographic method was developed that used a reverse phase disposable cartridge cleanup and isocratic chromatography with a reverse phase octadecylsilica column and a UV detector set at 212 nm. Recovery of cyclosporin A from spiked rice samples (mg/g range) was 85%.

摘要

本文介绍了一种测定和定量大米中环孢菌素A(一种环肽霉菌毒素)的简单方法。接种多孢木霉(Link ex Pers.)的大米在培养4周后用二氯甲烷提取。通过开放床凝胶过滤柱色谱法(LH - 20,乙腈)从提取物中分离环孢菌素A,并用薄层色谱法和与标准品反相液相色谱共洗脱进行监测。开发了初步的薄层色谱方法。环孢菌素A通过碘检测,部分酸水解后通过茚三酮和紫外光检测。开发了一种液相色谱方法,该方法使用反相一次性柱净化以及在反相十八烷基硅胶柱和设置在212 nm的紫外检测器上进行等度色谱分析。从加标大米样品(毫克/克范围)中环孢菌素A的回收率为85%。

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