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作 者:王素娟 段海波 秦云华 范多青 王岚 李响丽 赵敏 WANG Su-juan;DUAN Hai-bo;QIN Yun-hua;FAN Duo-qing;WANG Lan;LI Xiang-li;ZHAO Min(China tobacco yunnan industrial Co.,Ltd,Kunming 650231,China)
机构地区:[1]云南中烟工业有限责任公司,云南昆明650231
出 处:《化学研究与应用》2018年第3期415-420,共6页Chemical Research and Application
摘 要:建立了一种快速、灵敏、选择性强的超高效液相色谱-串联质谱法同时测定食用香精香料中的1种甜味剂和6种防腐剂的分析方法。样品经含有内标(水杨酸-D4)的甲醇/水(7/3)振荡提取,ACQUITY UPLC?BEH C18色谱柱(100 mm×2.1 mm,1.7μm)分离,流动相为甲醇和0.05%甲酸水溶液,梯度洗脱,以电喷雾负离子多反应监测(MRM)模式进行质谱分析。实验表明,7种目标物在线性范围内具有较好的线性关系,相关系数大于0.99,定量限(10S/N)在0.03 mg·kg-1~2.33 mg·kg-1之间,三水平回收率在87.6%~104.4%之间,相对标准偏差(n=6)在1.47%~4.89%之间。A rapid,sensitive and highly selective analytical method by ultra performance liquid chromatography/tandem mass Spectrometry(UPLCMS/MS)was developed for the simultaneous determination of one sweetener and six preservatives in edible essences and spices.The sample was extracted and oscillated by methanol/water(7/3)containing an internal standard(2-Hydroxybenzoic-3,4,5,6-d4 Acid),the UPLC separation was performed on an ACQUITY UPLCR BEH C18 column(100 mm×2.1 mm,1.7μm)with a linear gradient elution program of methanol and 005%formic acid aqueous solution as the mobile phase,electrospray ionization was applied and operated in the negative multiple reaction monitoting(MRM)mode.The results showed that the limits of quantitation(S/N>10)were in the range of 0.03 mg·kg-1~2.33 mg·kg-1,the three level recoveries were between 87.6%and104.4%with the relative standard deviations(n=6)of 147%~489%,the calibration curves showed good linearity for the seven analytes in their detection ranges,and the correlation coefficients(r2)were larger than 0.99
关 键 词:超高效液相色谱-串联质谱法 食用香精香料 甜味剂 防腐剂 测定
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