| 通过式固相萃取净化/UPLC-MS/MS法测定特殊医学用途配方食品中的13种非法添加化学成分 |
| 点此下载全文 |
|
| 基金项目:浙江省食品药品监管系统科技计划项目(SP2018031) |
|
| 中文摘要:建立了特殊医学用途配方食品中非法添加的13种降糖类化学成分的通过式固相萃取净化/超高效液相色谱-串联质谱检测方法。样品用90%乙腈水溶液(含1%甲酸)提取后，提取液经Oasis PRiME HLB 固相萃取柱净化，以Waters ACQUITY UPLC BEH C18(150 mm×2.1 mm，1.7 μm)色谱柱分离，以甲醇-含0.1%甲酸的5 mmol/L乙酸铵溶液为流动相梯度洗脱，正离子模式电喷雾电离，配合多反应离子扫描(MRM)定性定量分析目标化合物。考察了提取剂用量、甲酸及乙腈含量对加标回收率的影响，优化了主要的影响因素和实验条件。结果表明：13种化合物在2~100 μg/L范围内线性关系良好，相关系数r2≥0.995 1；方法回收率为80.9%~102.8%；定量下限为0.3~1.0 μg/kg。该方法前处理简单，回收率高，重现性好，可作为降糖类特殊医学用途配方食品中非法添加降糖类化学成分的有效检测方法。 |
| 中文关键词:超高效液相色谱-串联质谱 通过式固相萃取 特殊医学用途配方食品 降糖 |
| |
| Determination of 13 Ingredients Illegally Added in Formulated Foods on Special Medical Purposes by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry with Pass-through Solid Phase Extraction |
|
|
| Abstract:An ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was developed for the determination of 13 anti-diabetic ingredients illegally added in formulated foods on special medical purposes.Samples were extracted with 90% acetonitrile containing 1% formic acid,and then purified with an Oasis PRiME HLB column.The extraction was on a Waters ACQUITY UPLC BEH C18(150 mm×2.1 mm，1.7 μm) column with methanol-5 mmol/L ammonium acetate solution containing 0.1% formic acid as mobile phases by gradient elution.The analysis on the analyte was performed by UPLC-MS/MS under positive electrospray ionization in multiple reaction monitoring(MRM) mode,Effects affecting the recoveries such as dosage of extractant,formic acid and acetonitrile in cleaning-up agent were investigated.The main influence factors and analytical conditions were modified.Results showed that there were good linear relationships for 13 ingredients in the concentration range of 2-100 μg/L with their correlation coefficients(r2) no less than 0.995 1.The recoveries at three concentration levels ranged from 80.9% to 102.8% with LOQs of 0.3-1.0 μg/kg.With simple pretreatment,high recovery and good reproducibility,the developed method was suitable for the determination of 13 anti-diabetic ingredients illegally added in formulated foods on special medical purposes. |
| Key Words:ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) dispersive solid phase extraction foods for special medical purpose anti-diabetic |
| 引用本文：励炯,邱红钰，贾彦博，王红青，李玮.通过式固相萃取净化/UPLC-MS/MS法测定特殊医学用途配方食品中的13种非法添加化学成分[J].分析测试学报,2018,37(3):307-312. |
| 摘要点击次数: 1985 |
| 全文下载次数: 875 |
| 查看全文 下载PDF阅读器 |
|
|
