Knowledge Resource Center for Ecological Environment in Arid Area
超高效液相色谱-串联质谱法检测螺旋藻保健品中7种微囊藻毒素 | |
其他题名 | Determination of 7 microcystins in Spirulina health food products by ultra performance liquid chromatography-tandem mass spectrometry |
李兵; 刘伟; 范赛; 赵榕; 吴国华 | |
来源期刊 | 色谱
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ISSN | 1000-8713 |
出版年 | 2012 |
卷号 | 30期号:6页码:584-589 |
中文摘要 | 采用固相萃取净化结合超高效液相色谱-串联质谱法(UPLC-MS/MS)测定了螺旋藻保健品中7种微囊藻毒素(MCs)。螺旋藻保健品经70%(体积分数)的甲醇超声提取,冷冻离心沉淀杂质后,经HLB柱净化。在WatersACQUITY UPLC~? BEH C18色谱柱上以乙腈和0.2 mmo l/L乙酸铵水溶液为流动相进行梯度洗脱分离,采用电喷雾离子源正离子模式进行多反应离子监测,外标法定量。7种MC在线性范围内线性关系良好(相关系数(r)不小于0.995);检出限为6.7~33.3mug/kg,定量限为20.0~100.0mug/kg。各分析物在阴性螺旋藻保健品中的加标回收率在87.5%~97.9%之间,相对标准偏差(RSD)在1.6%~6.9%之间。该方法准确可靠,灵敏度高,可用于螺旋藻保健品中MC污染的确证定性、定量检测。 |
英文摘要 | Ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) combined with solid phase extraction(SPE) has been developed for the determination of 7 microcystins(MCs) in Spirulina health food products.The sample was extracted by 70%(v/v) methanol.The lipid substances were isolated by centrifugation under freezing condition,and then followed by clean-up with a Waters Oasis HLB solid phase extraction cartridge.The separation was performed on a Waters ACQUITY UPLCBEH C18 column with gradient elution using acetonitrile and 0.2 mmol/L ammonium acetate.The electrospray ionization(ESI) source in positive ion mode was used for multiple reaction monitoring(MRM).The external standard method was used for the quantification.The linear ranges for 7 MCs were 20-400 mug/kg,and the correlation coefficients were not less than 0.995.The limits of detection were 6.7-33.3 mug/kg.The limits of quantification were 20.0-100.0 mug/kg.The recoveries of the 7 MCs spiked in blank Spirulina samples ranged from 87.5% to 97.9% with the relative standard deviations of 1.6%-6.9%.The results demonstrated that the method is easy,fast,sensitive,and suitable for the confirmation and quantification of the 7 MCs in Spirulina samples. |
中文关键词 | 固相萃取 ; 超高效液相色谱-串联质谱 ; 微囊藻毒素 ; 螺旋藻保健品 |
英文关键词 | solid phase extraction(SPE) ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) microcystins(MCs) Spirulina health food products |
语种 | 中文 |
国家 | 中国 |
收录类别 | CSCD |
WOS类目 | CHEMISTRY ANALYTICAL |
WOS研究方向 | Chemistry |
CSCD记录号 | CSCD:4568728 |
资源类型 | 期刊论文 |
条目标识符 | http://119.78.100.177/qdio/handle/2XILL650/228385 |
作者单位 | 北京市疾病预防控制中心营养与食品卫生所, 北京 100013, 中国 |
推荐引用方式 GB/T 7714 | 李兵,刘伟,范赛,等. 超高效液相色谱-串联质谱法检测螺旋藻保健品中7种微囊藻毒素[J],2012,30(6):584-589. |
APA | 李兵,刘伟,范赛,赵榕,&吴国华.(2012).超高效液相色谱-串联质谱法检测螺旋藻保健品中7种微囊藻毒素.色谱,30(6),584-589. |
MLA | 李兵,et al."超高效液相色谱-串联质谱法检测螺旋藻保健品中7种微囊藻毒素".色谱 30.6(2012):584-589. |
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