超高效液相色谱-串联三重四极杆质谱法测定银杏叶保健食品中4’-O-甲基吡哆醇  

Determination of 4'-O-Methylpyridoxine in Ginkgo biloba Leaves Health Foods by A Validated Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：蒋迪尧 梅秀明 吴肖肖 JIANG Diyao;MEI Xiuming;WU Xiaoxiao(Key Laboratory of Biotoxin Analysis&Assessment for State Market Regulation,Nanjing Institute of Product Quality Inspection(Nanjing Institute of Quality Development and Advanced Technology Application),Nanjing 210019,China)

机构地区：[1]国家市场监管重点实验室(生物毒素分析与评价),南京市产品质量监督检验院(南京市质量发展与先进技术应用研究院),江苏南京210019

出　　处：《食品科技》2024年第5期328-333,共6页Food Science and Technology

基　　金：国家重点研发计划项目(2023YFF1105102);江苏省市场监管局科技计划项目(KJ2022070);国家市场监管总局科技计划项目(2022MK160);国家市场监管总局技术保障专项项目(2023YJ18)。

摘　　要：基于超声辅助萃取结合超高效液相色谱-串联质谱法建立检测银杏叶保健食品中4’-O-甲基吡哆醇(4’-O-methylpyridoxine,MPN)的高灵敏分析方法。对样品采用纯水超声辅助萃取,探究提取时间对目标物提取效率的影响。目标物经ACQUITY-UPLC BEH-C_(18)(2.1 mm×100 mm,1.7μm)色谱柱分离,以甲醇和水为流动相梯度洗脱,流速0.25 mL/min,柱温30℃。电喷雾离子源正离子多反应监测模式采集,外标法定量。纯水超声辅助萃取10 min,提取效果最佳。MPN在1~500ng/mL质量浓度范围内线性关系良好,相关系数r为0.9996,方法检出限为0.2μg/kg,定量限为0.7μg/kg,加标回收率为97.49%~100.42%,方法重复性相对标准偏差为0.27%。在实际样品检测中,检出样品MPN含量为0.78~80.34 mg/kg。建立的超声辅助萃取结合超高效液相色谱-串联质谱法操作简单、灵敏度与准确性高,选择性好,适用于银杏叶保健食品中MPN的高灵敏定量检测。A highly sensitive analytical method for determination of 4'-O-methylpyridoxine(MPN) in Ginkgo biloba leaves health foods was established based on ultra-high performance liquid chromatographytandem mass spectrometry(UPLC-MS/MS) with ultrasound assisted extraction.Ultrasound assisted extraction of samples by pure water was used.Effect of different extraction time on efficiency extraction of target compound was investigated.The target compound was separated on an ACQUITY-UPLC BEH-C_(18)(2.1 mm × 100 mm,1.7 μm) chromatographic column using a gradient elution of methanol and water at a flow rate of 0.25 mL/min and a column temperature of 30℃.Electrospray ionization(ESI) in positive ion multiple reaction monitoring(MRM) mode was used for detection,and external standard method was used for quantification.The optimal extraction time was found to be 10 min for ultrasound-assisted extraction with pure water.The MPN showed a good linear relationship within the range of 1–500 ng/mL with a correlation coefficient(r) of 0.9996.The limit of detection(LOD) of the method was 0.2 μg/kg and the limit of quantification(LOQ) was 0.7 μg/kg.The recoveries of the target substance were 97.49%–100.42%,and the relative standard deviation(RSD) of method repeatability was 0.27%.The MPN contents in actual samples were 0.78–80.34 mg/kg.The established method was simple to operate,had high sensitivity and accuracy and good sensitivity.It was suitable for the quantitative determination of MPN in Ginkgo biloba leaves health foods.

关 键 词：4’-O-甲基吡哆醇 超高效液相色谱-串联质谱 银杏叶保健食品 

分 类 号：TS207.3[轻工技术与工程—食品科学]