摘要
本文建立了以超高效液相色谱串联质谱法(UPLC-MS)测定低聚原花青素(OPCs)的方法。样品中原花青素在含高铁离子的酸性乙醇溶液中经密闭高温反应后生成氰定离子,通过含1%甲酸,28%水甲醇组成的流动相(72∶28,v/v)经Zorbax Eclipse Plus C18反相色谱柱(2.1 mm×50 mm,1.8μm)分离,采用大气压电喷雾离子源(ESI)在选择离子监测(SIM)模式下以质荷比为287(m/z)的氰定正离子进行检测,并以美国药典(USP)低聚原花青素标准品进行定量。结果显示原花青素在0.2×10^(-6)~2×10^(-6) g/mL的浓度范围内呈良好线性关系,相关系数大于0.999,三个不同浓度水平的平均加标回收率在98%~104%之间,相对标准偏差(RSD)小于5%,此方法具有较高的精密度和准确度。该液质联用方法同时对比了不同标准品之间的差异,当采用低聚原花青素标准品时将有助于保证产品中原花青素测定结果的一致性。
An ultra-performance liquid chromatography(UPLC)with mass spectrometry method was developed for determination of oligomeric proanthocyanidins(OPCs).Proanothocyanidins in the samples was reacted in acidified ethanol containing high iron ions under closed high temperature condition to generate cyanide ions,cyanide ions were separated by Zorbax Eclipse Plus C18 reverse phase chromatographic column(2.1 mm×50 mm,1.8μm)with mobile phase(72∶28,v/v)consisting of 1%formic acid and 28%methanol in water.Electrospray ionization(ESI)equipped with selected ion monitoring mode was utilized to determine a positive cyanide ion with a mass charge ratio of 287(m/z),and total proanothocyanidns content was quantitated by a USP certified OPCs reference standard.Excellent correlation coefficients of the linear curve of proanothocyanidins was achieved(R>0.999)within the range of 0.2×10^(-6)~2×10^(-6 )g/mL,the average spike recovery at three different concentration levels was found to be within the range of 98%~104%,and RSD was less than 5%,demonstrated good precision and accuracy of the method.This study also found that different sources of reference standards resulted in different yielding rate of cyanidin,using oligomeric proanthocyanidin standards will help to ensure the consistency of proanthocyanidin determination results in the products.
作者
李建珍
顾文
周亮
LI Jianzhen;GU Wen;ZHOU Liang(Herbalife(China)Health Products Co.,Ltd.,Suzhou 215021)
出处
《中国食品添加剂》
CAS
2024年第2期263-271,共9页
China Food Additives
