液相色谱-串联质谱法测定海参和海胆中的单唾液酸神经节苷脂  

Determination of monosialogangliosides in sea cucumbers and sea urchins usingliquid chromatography tandem mass spectrometry

作　　者：丛培旭[1] 李兆杰[1] 徐杰[1] 于槚槚[1] 常耀光[1] 薛长湖[1] 

机构地区：[1]中国海洋大学食品科学与工程学院,山东青岛266003

出　　处：《色谱》2013年第5期399-403,共5页Chinese Journal of Chromatography

基　　金："十二五"国家科技支撑计划项目(2012BAD33B07);宁波市重大科技攻关计划项目(2012C10019);长江学者和创新团队发展计划项目;中央高校基本科研业务费实验室研究基金项目(201251009)

摘　　要：建立液相色谱－四极杆串联质谱法定量检洲海参和海胆中单唾液酸神经节苷脂的分析方法，采川Sven－nerhohu法从海肌或海参样中提取神经节苷脂，经c8引相萃取柱净化，采用APS－2NH，柱（150mill×2．1mｍ，3μm）．以已腑和50mmol／L乙酸铵溶液（pH5．6）为流动相．梯度洗脱。样品中每种成分的定量在多反应监测模式下进行、该方法具有极高的灵敏度，定量限可低至纳克级。非硫酸酯化单唾液酸神经节汗脂（NMG）和硫酸哺化单唾液酸神经节苷脂（SMG）在1～40ng进样垃范剧内毕现良好的线性关系；定昔结果显示所测海参样品中美国红参的NMG龠艟最商，海胆样品中紫海胆的SMG含菌最高；海胆中总的单唾液酸神经节苷脂含量（4．30～6．40mg／g）明显高于各海参样品（8～J31μg／g）。该方法稳定可靠。An approach based on liquid chromatography-tandem mass spectrometry was devel- oped for the quantification of monosialogangliosides （MG） in sea cucumbers and sea urchins. The gangliosides of sea cucumbers and sea urchins were extracted according to the Svenner- hohn method and cleaned up by C8 solid phase extraction column. The extracts were separated on an APS-2 NH, column （ ｜ 50 mm x 2. l ram, 3 μm） with the mobile phases of acetonitrile and 50 mmol/L ammonium acetate （pH 5.6） under gradient elution. Multiple reaction monitoring （MRM） was performed for quantification of each analyte in the samples. The method was capable to distinguish gangliosides with different types of sialic acid in a single run. The limit of quantification was 0. 22 ng for nonsulfated monosialoganglioside （NMG） and 0. 29 ng for sulfat- ed monosialoganglioside （ SMG）, and the linear range was I - 40 ng for both compounds. Only NMG was detected in sea cucumbers while both NMG and SMG were detected in sea urchins. Quantification results suggested that NMG was most abundant in Parastichopus californicus among all the sea cucumbers detected and SMG was most abundant in Anthocidaris crassispi- na among all the sea urchins. The contents of MGs in sea urchins （4.30 - 6.40 mg/g） were much higher than those in sea cucumbers （8 - 131 μg/g）. The method is suitable for the quan- tification of monosialogangliosides in sea urchins and sea cucumbers.

关 键 词：液相色谱-串联质谱 多反应监测 单唾液酸神经节苷脂 海参 海胆 

分 类 号：O658[理学—分析化学]