高效液相色谱法测定南极磷虾及其制品中虾青素的含量

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~20.999);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。

Determination of astaxanthin in Antarctic krill and its products by high performance liquid chromatography

Objective To establish a method for the determination of astaxanthin in Antarctic krill and its products by high performance liquid chromatography (HPLC). Methods Samples were dehydrated with anhydrous MgSO4, extracted with acetone, cleaned by 200 mg primary secondary amine (PSA) for dispersive solid-phase extraction, saponified by 0.02 mol/L NaOH methanol for 12~16 h, and separated on a YMC-Carotenoid C30 column using methanol, methyl tert-butyl ether and 1% phosphoric acid as mobile phase for gradient elution, and then detected by ultraviolet detector. Results The limits of quantitation for astaxanthin in Antarctic krill and krill powder were 2.5 and 5 mg/kg, respectively. The trans-astaxanthin had a good linearity (r2>0.999) in the range of 0.1~10 mg/L. The spiked recoveries were between 77.9 % and 91.3 %, with relative standard derivations (RSDs) from 3.42 % to 8.75 %. The differences of astaxanthin content from different krill powder products were obvious. Conclusion The developed method is simple and accurate, and is suitable for detection of astaxanthin in Antarctic krill and its products.