摘要
为更好地测定水产品的鲜度,建立了亲水性色谱测定水产品中6种ATP关联化合物的方法,确定以乙腈-2.0 mmol/L KH2PO4(体积比80∶20)为流动相等度洗脱,采用BEH Amide(4.6 mm×250 mm,5μm)色谱柱,柱温35℃,流速1.0 mL/min,波长254 nm进行检测。结果表明:6种ATP关联化合物在16 min内完全分离,在5.0~200.0μmol/L范围内线性关系良好,相关系数在0.9950~0.9999之间,保留时间相对标准偏差0.5%~2.0%,加标回收率在82.0%~108.2%,相对标准偏差0.8%~6.4%。该方法重现性好,准确度高,可用于水产品中6种ATP关联化合物的测定分析。
In this work, the use of hydrophilic-interaction liquid chromatography(HILIC) was studied in order to determine freshness of aquatic product. A new, sensitive and accurate method for the simultaneous determination of six kinds of ATP related compounds(ATP, ADP, AMP, IMP, HxR, Hx) in fish was developed and validated. The detection limit, the linearity and the repeatability of this method were also determined. The compounds were separated by using BEH Amide column(4.6 mm × 250 mm, 5 μm). The mobile phase was acetonitrile and water(2 mmol/L KH2 PO4) in a ratio of 80 ∶ 20(V/V), which was eluted at an isocratic flow rate of 1.0 mL/min. The column temperature was 35 ℃,detection wavelength was 254 nm. The results showed that, six kinds of ATP related compounds were separated completely within 16 min. The linearity was good in the range of 5.0-200.0 μmol/L, the correlation coefficient range from0.9950 to 0.9999. Relative standard deviations(RSDs) of retention time range from 0.5% to 2.0%. Recovery study was conducted at three different fortification levels and the average ranged from 82.0% to 108.2% for all of the studied compounds with RSDs within 0.8%-6.4%. The method has a high accuracy and reproducibility in the determination of six ATP related compounds in aquatic product.
作者
张慧恩
王彩霞
杨华
Zhang Huien;Wang Caixia;Yang Hua(College of Biological and Environmental Sciences,Zhejiang Wanli University,Ningbo 315100,Zhejiang;Ningbo Yu Fang Tang Biological Science and Technology Co.,Ltd.,Ningbo 315100,Zhejiang)
出处
《中国食品学报》
EI
CAS
CSCD
北大核心
2019年第4期266-271,共6页
Journal of Chinese Institute Of Food Science and Technology
基金
国家科技部星火计划项目(2015GA701038)
浙江省公益技术研究农业项目(2016C32068)
浙江省"生物工程"一流学科课题(ZS2018002)
宁波市科技富民项目(2016C10009)
关键词
亲水性色谱
ATP关联化合物
K值
hydrophilic interaction liquid chromatography
ATP related compounds
K value