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机构地区:[1]大连理工大学化工学院,辽宁大连116023 [2]大连市产品质量监督检验所,辽宁大连116021
出 处:《色谱》2010年第6期590-595,共6页Chinese Journal of Chromatography
基 金:国家标准制(修)订计划(No.20068134-T-469)
摘 要:建立了辣椒粉及辣椒油中7种罗丹明染料的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。样品经正己烷或甲醇-水(体积比为1∶1)溶液提取后,经固相萃取(SPE)柱净化,采用SB-C18柱分离,以乙腈和水(含体积分数为0.1%的甲酸)为流动相进行梯度洗脱,采用正离子模式质谱检测,在多反应监测(MRM)模式下进行定性定量测定。7种罗丹明类染料在0.000 5~1.0mg/L质量浓度范围内线性关系良好,相关系数(r2)均大于0.997;方法的检出限分别为0.21~51μg/kg(辣椒粉)和0.19~25μg/kg(辣椒油);方法的回收率为85.0%~106.0%,日内及日间相对标准偏差均小于20%。该方法简单、灵敏度高、分析时间短,适用于辣椒粉和辣椒油中7种罗丹明染料的同时测定。A credible method was developed for the simultaneous determination of 7 rhodamine dyes in hot chili products based on high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The samples were extracted with hexane or methanol-water(1∶1,v/v) and then cleaned up by a solid phase extraction cartridge.The target analytes were separated on an SB-C18 column with gradient elution using acetonitrile and water(containing 0.1%(v/v) formic acid for both) as mobile phases.The identification and quantification were achieved by using ESI-MS/MS in positive ion mode and with multiple reaction monitoring(MRM).The linear ranges were from 0.000 5 to 1.0 mg/L with the correlation coefficients(r^2) above 0.997 for all the 7 rhodamine dyes.The limits of detection(LOD) in chili powder and chili oil were from 0.21 to 51 μg/kg and 0.19 to 25 μg/kg,respectively.The relative standard deviations of intra-day and inter-day were both less than 20%.The recoveries of the method were between 85.0% and 106%.The method is simple,rapid,highly sensitive and suitable for the simultaneous determination of 7 rhodamine dyes in foods.
关 键 词:高效液相色谱-串联质谱 罗丹明染料 辣椒粉 辣椒油
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