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苹果汁中展青霉素的注射器-滤芯固相萃取法

Syringe-cartridge solid-phase extraction method for patulin in apple juice.

作者信息

Eisele Thomas A, Gibson Midori Z

机构信息

Tree Top Inc., PO Box 248, 111 S. Railroad Ave, Selah, WA 98942, USA.

出版信息

J AOAC Int. 2003 Nov-Dec;86(6):1160-3.

Abstract

A syringe-cartridge solid-phase extraction (SPE) method was developed for determination of patulin in apple juice. A 2.5 mL portion of test sample was passed through a conditioned macroporous SPE cartridge and washed with 2 mL 1% sodium bicarbonate followed by 2 mL 1% acetic acid. Patulin was eluted with 1 mL 10% ethyl acetate in ethyl ether and determined by reversed-phase liquid chromatography using a mobile phase consisting of 81% acetonitrile, 9% water, and 10% 0.05M potassium phosphate buffer, pH 2.4. Recoveries averaged 92% and the relative standard deviation was 8.0% in test samples spiked with 50 ng/mL patulin. The method appears to be applicable for monitoring apple juice samples to meet the U.S. Food and Drug Administration compliance action level of 50 microg/kg in an industrial quality assurance laboratory environment.

摘要

建立了一种用于测定苹果汁中展青霉素的注射器-柱式固相萃取(SPE)方法。取2.5 mL测试样品通过已活化的大孔SPE柱,先用2 mL 1%碳酸氢钠洗涤,再用2 mL 1%乙酸洗涤。用1 mL 10%乙酸乙酯的乙醚溶液洗脱展青霉素,并用反相液相色谱法测定,流动相由81%乙腈、9%水和10% 0.05M磷酸钾缓冲液(pH 2.4)组成。在添加了50 ng/mL展青霉素的测试样品中,回收率平均为92%,相对标准偏差为8.0%。该方法似乎适用于在工业质量保证实验室环境中监测苹果汁样品,以符合美国食品药品监督管理局50 μg/kg的合规行动水平。

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