建立基于通过式固相萃取净化检测特殊医学用途配方乳粉中姜黄素的超高效液相色谱串联质谱检测方法.样品经80％乙腈提取,通过Oasis PRiME HLB固相萃取柱净化后,以乙腈-0.1％甲酸溶液作为流动相,在acquity UPLC HSS T3色谱柱上进行梯度洗脱,经超高效液相色谱仪进行分离后,通过电喷雾正离子模式电离,多反应监测模式进行检测分析,外标法定量.对目标物进行稳定性研究,对样品中目标物提取、净化方式、色谱分离条件、质谱条件等关键因素进行了优化.结果表明,3种姜黄素类化合物在25～2 500 ng/mL范围内线性关系好,相关系数高于0.99,加标回收率在87.9％～102.8％之间,精密度在1.31％～4.94％之间,3种姜黄素类化合物的检出限为10 μg/kg,定量限为25 μg/kg.该方法定性定量结果准确、稳定性好、灵敏度高,能够对特殊医学用途配方乳粉中姜黄素类化合物进行定性分析与定量检测.
Abstract
A method for the determination of curcumin in formula milk powder for special medical purposes by ultra performance liquid chro-matography tandem mass spectrometry(UPLC-MS/MS)was established.Samples were extracted by 80％acetonitrile and purified by Oasis PRiME HLB.After the membrane was passed,the acetonitrile-0.1％formic acid solution was used as mobile phase to carry out gradient elution on the acquity UPLC HSS T3 chromatographic column.After separation by UPLC,it was detected by electrospray ionization mode ionization,multiple reaction monitoring mode,and quantified by external standard method.The stability of the targets was studied,and the key factors of pre-treatment were optimized,such as extraction solvent,purification,the separation effects of different chromatographic columns,and mobile phase conditions were investigated.The results showed that the three curcumin compounds in the range of 25-2 500 ng/mL,the correlation coefficient was greater than 0.99.The recoveries were in the range of 87.9％-102.8％and the precision was in the range of 1.31％-4.94％.The limit of detec-tion for the three curcumins was 10μg/kg,the limit of quantification for the three curcumins was 25 μg/kg.The method was accurate,stable and sensitive,and could be used for qualitative and quantitative analysis of curcumin compounds in formula milk powder for special medical purposes.
关键词
姜黄素类化合物/Oasis/PRiME/HLB/特殊医学用途配方乳粉/液相色谱串联质谱法
Key words
curcumin compounds/Oasis PRiME HLB/formula milk powder for special medical purposes/UPLC-MS/MS
维普
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