离子液体-K2HPO4超声双水相萃取预富集-高效液相色谱法测定水产品中组胺含量
HPLC Determination of Histamine in Fishery Products with Pre-enrichment by Ultrasonic Ionic Liquid-K2HPO4 Bi-aqueous Phase Extraction
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摘要: 样品经高氯酸溶液提取,丹磺酰氯衍生化,于离子液体1-丁基-3-甲基咪唑溴盐和磷酸氢二钾组成的双水相体系中进行萃取。待测物在XDB C18色谱柱上分离,以0.02 mol·L-1乙酸铵-乙腈混合液为流动相进行梯度洗脱,于波长254 nm处进行紫外检测。组胺的质量浓度在0.10~2.0 mg·L-1范围内呈线性,测定下限(10S/N)为0.05 mg·L-1。加标回收率在95.0%~103%之间,日内和日间相对标准偏差(n=6)分别在2.8%~6.1和4.8%~7.7%之间。Abstract: Histamine in the sample was extracted with CHlO4 solution and derivatized with dansyl chloride. The derivate in the mixture was then separated from the matrix by a binary aqueous phase ultrasonic extraction with an extractant system composed of ionic liquid 1-butyl-3-methylimidazolium bromide and K2HPO4. The analyte in the extract was then separated on XDB C18 column with mixtures of 0.02 mol·L-1 NH4OAc solution and acetonitrile (mixed in various ratios) as mobile phase in gradient elution. Linearity range for histamine was obtained between 0.10-2.0 mg·L-1, and the lower limit of determination (10S/N) was 0.05 mg·L-1. Recovery was tested by standard addition method, giving results ranged from 95.0% to 103%. Values of RSD′s (n=6) (intra-day and inter-day) found were in the ranges of 2.8%-6.1% and 4.8%-7.7% respectively.