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首页> 美国卫生研究院文献>Molecules >Determination of 4-Hexylresorcinol in Shrimp Samples by Solid Phase Extraction Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
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Determination of 4-Hexylresorcinol in Shrimp Samples by Solid Phase Extraction Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

机译：固相萃取超高效液相色谱-串联质谱法测定虾样品中的4-己基间苯二酚

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摘要

A method for the rapid determination of 4-hexylresorcinol (4-HR) residue in shrimp by solid phase extraction (SPE) ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. 4-HR was extracted twice with methanol, and the extract was formulated into methanol-water solution (1:1). After being cleaned up and concentrated by a PRIME HLB solid phase extraction column, the sample was analyzed by UPLC-MS/MS and quantitatively determined by an external standard method. The separation was performed with a gradient system consisting of water and acetonitrile as the mobile phase. Monitoring was performed by electrospray ionization (ESI) in negative ion mode using multiple ion reaction monitoring (MRM). Good linearity was obtained in the concentration range of 1.0–100.0 μg/L, with correlation coefficients larger than 0.999. The limit of detection (LOD) was 0.25 μg/kg and the limit of quantification (LOQ) was 0.80 μg/kg. The average recoveries of 4-HR at spiked concentrations of 2.40, 6.40 and 16 μg/kg ranged from 81.35% to 94.68% with the relative standard deviations (n = 6) from 3.57% to 6.86%. The results showed that the method is simple, fast, sensitive, reliable, and reproducible; thus, it could be used as a rapid confirmation and quantitative analysis method of 4-HR residue in aquatic products.
机译：建立了固相萃取（SPE）超高效液相色谱-串联质谱法（UPLC-MS / MS）快速测定虾中4-己基间苯二酚（4-HR）残留量的方法。将4-HR用甲醇萃取两次，然后将萃取液配制成甲醇-水溶液（1：1）。在通过PRIME HLB固相萃取柱净化并浓缩后，通过UPLC-MS / MS分析样品，并通过外标方法定量测定。使用由水和乙腈组成的梯度系统作为流动相进行分离。使用多离子反应监测（MRM）以负离子模式通过电喷雾电离（ESI）进行监测。在1.0–100.0μg/ L的浓度范围内可获得良好的线性，相关系数大于0.999。检测极限（LOD）为0.25μg/ kg，定量极限（LOQ）为0.80μg/ kg。加标浓度为2.40、6.40和16μg/ kg时4-HR的平均回收率在81.35％至94.68％之间，相对标准偏差（n = 6）从3.57％至6.86％。结果表明，该方法简便，快速，灵敏，可靠，可重复。因此，可作为水产品中4-HR残留量的快速确认和定量分析方法。

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