超高效液相色谱法测定水产品保鲜剂中4-己基间苯二酚的含量

摘要

建立一种准确测定保鲜剂样品中4-己基间苯二酚的超高效液相色谱-荧光色谱的检测方法.色谱条件为色谱柱(2.1 nm×150 mm,1.7 μm),乙腈-水(70:30)为流动相,激发波长280 nm,发射波长310 nm,流速为0.3 mL/min,柱温为35℃.样品通过乙腈提取,提取液经超声后高速离心,然后通过0.22 μm有机相微孔滤膜过滤后上机进样,进行超高效液相色谱-荧光色谱分析.方法在0.10~20.00 μg/mL(R=0.999)呈良好的线性关系,其回收率为83.75%~100.70%,相对标准偏差小于5.76%(n=6),检出限为2.0 mg/kg.利用本方法对市售5种保鲜剂进行了分析,发现其中一种含有4-己基间苯二酚,另外4种均为阴性样品.本方法快速、准确、灵敏度高,可广泛用于保鲜剂中4-己基间苯二酚含量的分析测定.%A method for the determination of 4-hexylresorcinol in the samples of aquatic preservative was established by ultra performance liquid chromatography-fluorescence spectroscopy was established (UPLC-FLD). The chromatographic column conditions were as follows: (2.1 nm×150 mm, 1.7 μm), acetonitrile-water (70:30) as the mobile phase. The excitation wavelength was 280 nm, the emission wavelength was 310 nm, the flow rate was 0.3 mL/min and the column temperature was 35 ℃. The sample was extracted with acetonitrile, and the extract was centrifuged at high speed after ultrasonic irradiation. Then, the supernatant were filtered through a 0.22 μm organic phase micro membrane and then injected into fluorescence spectroscopy (FLD) to analysis.The standard solution of 4-hexylresorcinol was in the range of 0.10-20.00 μg/mL(R=0.999)showed a good linear relationship, the average recoveries were 83.75%-100.70% and the relative standard deviations were less than 5.76%(n=6), the detection limit was 2.0 mg/kg. The results showed that only one of the five kinds of preservatives contained 4-hexylresorcinol and the other four were negative samples. This method is rapid,accurate and sensitive,and it is suitable for determination of content in preservative.