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首页> 外文期刊>Journal of Agricultural and Food Chemistry >Simultaneous determination of ochratoxin A and cyclopiazonic, mycophenolic, and tenuazonic acids in cornflakes by solid-phase microextraction coupled to high-performance liquid chromatography
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Simultaneous determination of ochratoxin A and cyclopiazonic, mycophenolic, and tenuazonic acids in cornflakes by solid-phase microextraction coupled to high-performance liquid chromatography

机译：固相微萃取-高效液相色谱法同时测定玉米片中的ra曲霉毒素A和环吡唑啉酸，霉酚酸和tenuazonic酸

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摘要

A solid-phase microextraction (SPME) method, coupled to liquid chromatography with diode array UV detection (LC-UV/DAD), for the simultaneous determination of cyclopiazonic acid, mycophenolic acid, tenuazonic acid, and ochratoxin A is described. Chromatographic separation was achieved on a propylamino-bonded silica gel stationary phase using acetonitrile/methanol/ammonium acetate buffer mixture (78:2:20, v/v/v) as mobile phase. SPME adsorption and desorption conditions were optimized using a silica fiber coated with a 60 mum thick polydimethylsiloxane/divinylbenzene film. Estimated limits of detection and limits of quantitation ranged from 3 to 12 ng/mL and from 7 to 29 ng/mL, respectively. The method has been applied to cornflake samples. Samples were subjected to a preliminary short sonication in MeOH/2% KHCO3 (70:30, v/v); the mixture was evaporated to near dryness and reconstituted in 1.5 mL of 5 mM phosphate buffer (pH 3) for SPME followed by LC-UV/DAD. The overall procedure had recoveries (evaluated on samples spiked at 200 ng/g level) ranging from 74 +/- 4 to 103 +/- 9%. Samples naturally contaminated with cyclopiazonic and tenuazonic acids were found; estimated concentrations were 72 +/- 9 and 25 +/- 6 ng/g, respectively.
机译：描述了一种固相微萃取（SPME）方法，结合了带有二极管阵列紫外检测器（LC-UV / DAD）的液相色谱法，用于同时测定环吡唑酸，麦考酚酸，tenuazonic酸和曲霉毒素A。使用乙腈/甲醇/乙酸铵缓冲液混合物（78：2：20，v / v / v）作为流动相，在丙基氨基键合的硅胶固定相上实现色谱分离。使用涂有60微米厚的聚二甲基硅氧烷/二乙烯基苯薄膜的硅纤维优化SPME的吸附和解吸条件。估计的检测限和定量限分别为3至12 ng / mL和7至29 ng / mL。该方法已应用于玉米片样品。样品在MeOH / 2％KHCO3（70:30，v / v）中进行短暂的超声处理。将该混合物蒸发至几乎干燥，并在1.5 mL 5 mM磷酸盐缓冲液（pH 3）中重新配制用于SPME，然后进行LC-UV / DAD。整个过程的回收率（以加标浓度为200 ng / g的样品评估）为74 +/- 4至103 +/- 9％。发现了被环吡唑酸和tenuazonic酸自然污染的样品。估计浓度分别为72 +/- 9 ng / g和25 +/- 6 ng / g。

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