摘要
为构建葡萄中柠檬酸、苹果酸和酒石酸的高灵敏同步检测方法,本研究以拖尾因子为核心评价指标,系统评估了C18、T3、Amide、Diamond Hydride及亲水色谱(HILIC) 5种不同分离机制色谱柱的分离性能。结果表明:HILIC色谱柱结合体积分数0.6%甲酸水溶液-0.6%甲酸乙腈等度洗脱,通过抑制硅醇基电离、增强亲水作用,可使目标物拖尾因子优化至0.95~1.05,所建超高效液相色谱-串联质谱(UPLC-MS/MS)法的检出限为0.028~0.160mg/L,定量限为0.093~0.530 mg/L,加标回收率为81.61%~103.25%,相对标准偏差为1.65%~12.57%,10份阳光玫瑰葡萄样品的检测结果与文献报道范围一致。该方法首次将HILIC色谱柱应用于葡萄有机酸分析,成功实现葡萄中3种有机酸的高灵敏度同步检测,为亲水性有机酸的高通量检测提供了技术支撑。
A high-sensitivity method was established for the simultaneous detection of citric acid,malic acid,and tartaric acid in grapes.Using the tailing factor as the core evaluation index,we systematically evaluated the separation performance of five chromatographic columns with different separation mechanisms,namely C18,T3,Amide,Diamond Hydride,and HILIC columns.As a result,the HILIC column,by combination with a 0.6%formic acid aqueous solution-a 0.6%formic acid-acetonitrile isocratic elution system,could effectively provide symmetric peak(tailing factor:0.95-1.05)by suppressing silanol ionization and enhancing hydrophilic interactions.Such a UPLC-MS/MS method demonstrated the following:detection limits(LODs)of 0.028-0.160 mg/L,quantification limits(LOQs)of 0.093-0.530 mg/L,spiked recoveries of 81.61%-103.25%,and relative standard deviations(RSDs)of 1.65%-12.57%.The organic acid contents in 10 Shine Muscat grape samples were subsequently analyzed using our established method,and the resultant data were quite consistent with literature-reported ranges.As a pioneering application of HILIC columns for organic acid analysis in grapes,our highly sensitive simultaneous detection of the three target acids will provide robust technical support for high-throughput detection of hydrophilic organic acids.
作者
吴琴燕
李冬冬
梁红芳
郑翠
刘吉祥
王建华
陈露
饶斌
秦岭
赵来成
WU Qinyan;LI Dongdong;LIANG Hongfang;ZHENG Cui;LIU Jixiang;WANG Jianhua;CHEN Lu;RAO Bin;QIN Ling;ZHAO Laicheng(Central Laboratory of Zhenjiang Institute of Agricultural Sciences in Hill Area of Jiangsu Province,Zhenjiang 212400,China;Jiangsu Vocational College of Agriculture and Forestry,Zhenjiang 212400,China)
出处
《生物加工过程》
2025年第5期568-574,共7页
Chinese Journal of Bioprocess Engineering
基金
镇江市科技计划(SH2024111)
2025年度镇江市重大农业技术推广项目。
