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食品与发酵工业  2021, Vol. 47 Issue (16): 247-252    DOI: 10.13995/j.cnki.11-1802/ts.027529
  分析与检测 本期目录 | 过刊浏览 | 高级检索 |
QuEChERS-超高效液相色谱-串联质谱法检测腌腊肉中四种常用香料
李林竹1, 马凯1, 杨昌彪1, 黄永桥2, 王媛媛1, 范金旭1, 陶光灿1*
1(贵州省分析测试研究院,贵州 贵阳,550014)
2(贵州省检验技术研究应用中心,贵州 贵阳,550014)
Determination of four spices in cured meat samples by QuEChERS coupled with ultra-performance liquid chomatography-tandem mass spectrometry
LI Linzhu1, MA Kai1, YANG Changbiao1, HUANG Yongqiao2, WANG Yuanyuan1, FAN Jinxu1, TAO Guangcan1*
1(Guizhou Academy of Testing and Analysis, Guiyang 550014, China)
2(Guizhou Provincial Detection Technology Research and Application Center, Guiyang 550014, China)
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摘要 建立了QuEChERS-超高效液相色谱-串联质谱(ultra performance liquid chromatography-MS-MS,UPLC-MS/MS)检测腌腊肉中4种常用香料的方法。腌腊肉样品经甲酸-乙腈(体积比1∶999)溶液提取,无水硫酸钠、乙二胺-N-丙基硅烷和C18吸附剂净化,采用ZORBAX Eclipse Plus-C18反相色谱柱(100 mm×2.1 mm,1.8 μm)进行分离,流动相为乙腈-甲酸(体积比999∶1)水溶液,流速0.3 mL/min,柱温40 ℃,进样体积5.0 μL,电喷雾离子源电离,多反应监测模式采集信号,在正离子模式(ESI+)下完成定性定量分析。结果表明,4种香料在0.50~50 μg/L线性关系良好,相关系数(R2)均大于0.998;检出限(limit of detection,LOD)为0.5~5.0 μg/kg,定量限(limit of quantification,LOQ)为2.0~15.0 μg/kg。添加5、10、50 μg/kg 3个浓度水平,平均加标回收率为82%~103%,相对标准偏差(relative standard deviation,RSD)为1.6%~13.5%(n=6)。该方法简单快捷,回收率优良,灵敏度高,适用于腌腊肉样品中常用香料的检测。
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李林竹
马凯
杨昌彪
黄永桥
王媛媛
范金旭
陶光灿
关键词:  超高效液相色谱-串联质谱  QuEChERS  香料  腌腊肉    
Abstract: A method for simultaneous determination of four common spices in cured meat was developed using QuEChERS-ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample was first shaken with a formic acid-acetonitrile solution (volume ratio of 1∶999) and then carried out purification by the QuEChERS . ZORBAX Eclipse Plus-C18 reversed-phase chromatography column (100 mm×2.1 mm, 1.8 μm) was used for separation, the mobile phase was acetonitrile-0.1% formic acid aqueous solution(volume ratio of 999∶1)with the flow rate 0.3 mL/min and the column temperature at 40 ℃. And the sample volume was 5.0 μL,qualitative and quantitative analysis were performed in ion mode (ESI+) and multiple reaction monitoring mode. The results showed that all the four spices showed a good linear trend in the range of 0.5-50 μg/L and the correlation coefficient (R2) was greater than 0.998. The limits of detection (LODs) and the limits of quantification (LOQs) were 0.5-5.0 μg/kg and 2.0-15.0 μg/kg, respectively. The average recoveries were 82%-103%, with relative standard deviations of 1.6%-13.5% (n=6). The developed method is easy, accurate and sensitive, which is suitable for the effective detection of common spices in cured meat samples.
Key words:  ultra-performance liquid chromatography-tandem mass spectrometry    QuEChERS    spices    cured meat
收稿日期:  2021-04-06      修回日期:  2021-04-21                发布日期:  2021-09-10      期的出版日期:  2021-08-25
基金资助: 国家重点研发计划项目(2017YFC1601800);贵州省科技计划项目(黔科合平台人才[2018]5404);贵州省科技计划项目(黔科合重大专项字[2019]3011);贵州省科技计划项目(黔科合服企[2019]4001)
作者简介:  硕士,助理工程师(陶光灿正高级工程师为通讯作者,E-mail:tgcan@gzata.cn)
引用本文:    
李林竹,马凯,杨昌彪,等. QuEChERS-超高效液相色谱-串联质谱法检测腌腊肉中四种常用香料[J]. 食品与发酵工业, 2021, 47(16): 247-252.
LI Linzhu,MA Kai,YANG Changbiao,et al. Determination of four spices in cured meat samples by QuEChERS coupled with ultra-performance liquid chomatography-tandem mass spectrometry[J]. Food and Fermentation Industries, 2021, 47(16): 247-252.
链接本文:  
http://sf1970.cnif.cn/CN/10.13995/j.cnki.11-1802/ts.027529  或          http://sf1970.cnif.cn/CN/Y2021/V47/I16/247
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