离子交换固相萃取-超高效液相色谱-串联质谱法测定减肥食品中p-辛弗林和去氧肾上腺素
目的 建立混合强阳离子交换固相萃取法(mixed mode cation exchange solid-phase extraction,MCX)-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定减肥食品中p-辛弗林和去氧肾上腺素两种辛弗林含量的分析方法.方法 样品以50％甲醇为溶剂超声提取,离心后上清液经MCX固相萃取小柱净化,5％氨水甲醇洗脱,氮吹近干后初始流动相复溶,以HSS T3色谱柱(100 mm×2.1 mm,1.8μm)分离,以0.1％(V:V)...
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| Veröffentlicht in: | 食品安全质量检测学报 2022, Vol.13 (20), p.6692-6698 |
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| container_title | 食品安全质量检测学报 |
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| creator | 刘珈伶 |
| description | 目的 建立混合强阳离子交换固相萃取法(mixed mode cation exchange solid-phase extraction,MCX)-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定减肥食品中p-辛弗林和去氧肾上腺素两种辛弗林含量的分析方法.方法 样品以50％甲醇为溶剂超声提取,离心后上清液经MCX固相萃取小柱净化,5％氨水甲醇洗脱,氮吹近干后初始流动相复溶,以HSS T3色谱柱(100 mm×2.1 mm,1.8μm)分离,以0.1％(V:V)甲酸水溶液(含10 mmol/L乙酸铵)-乙腈作为流动相,进行梯度洗脱.在电喷雾正离子模式下,采用多反应监测(multiple reaction monitoring,MRM)模式,外标法定量.结果 p-辛弗林和去氧肾上腺素在1～100 ng/mL范围内与峰面积均成良好的线性,相关系数(r)均大于0.999.p-辛弗林和去氧肾上腺素的检出限均小于0.5μg/kg,定量限均小于1.0μg/kg,在咖啡、酵素粉、减肥茶和压片糖果4种减肥食品基质中1、2、10 ng/mL 3个水平下加标回收率为85.6％～110.4％,相对标准偏差均未超过5.0％(n=6).结论 该方法准确、可靠,可满足减肥食品中两种辛弗林的定量分析. |
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| title | 离子交换固相萃取-超高效液相色谱-串联质谱法测定减肥食品中p-辛弗林和去氧肾上腺素 |
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