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目的建立一种准确测定南极磷虾及其制品中虾青素含量的高效液相色谱方法。方法样品经无水MgSO_4去除水分,以丙酮提取目标物,200 mg N-丙基乙二胺(PSA)填料分散固相萃取净化,经0.02 mol/L氢氧化钠甲醇溶液皂化12~16 h后,经YMC-Carotenoid C30色谱柱分离,经甲醇、叔丁基甲基醚和1%磷酸水溶液的流动相进行梯度洗脱,紫外检测器测定。结果南极磷虾和南极磷虾粉中虾青素的定量限分别为2.5 mg/kg和5 mg/kg;在0.1~10 mg/L时,全反式虾青素的线性关系良好(r~2>0.999);该方法的加标回收率在77.9%~91.3%之间,相对标准偏差为3.42%~8.75%。不同磷虾粉产品中虾青素的含量差异很大。结论本方法操作简便、准确,适用于南极磷虾及其制品中虾青素含量的分析。
Objective To establish a method for the accurate determination of astaxanthin in Antarctic krill and its products by high performance liquid chromatography. Methods The samples were dehydrated with anhydrous MgSO_4, and the target compounds were extracted with acetone and dispersed with solid-phase extraction of 200 mg N-propyl ethylenediamine (PSA). After saponification with 0.02 mol / L sodium hydroxide in methanol for 12 to 16 h , Separated by YMC-Carotenoid C30 column and eluted with a mobile phase of methanol, tert-butyl methyl ether and 1% aqueous phosphoric acid, and detected by a UV detector. Results The limits of quantitation of astaxanthin in Antarctic krill and Antarctic krill were 2.5 mg / kg and 5 mg / kg, respectively. The linear correlation of astaxanthin at 0.1-10 mg / L was good (r ~ 2> 0.999). The spiked recoveries of this method ranged from 77.9% to 91.3% with relative standard deviations of 3.42% to 8.75%. Different krill products astaxanthin content varies widely. Conclusion The method is simple, accurate and suitable for the analysis of astaxanthin in Antarctic krill and its products.