食品工业2024,Vol.45Issue(7) :306-309.

UPLC-MS/MS法测定减肥类压片糖果中非法添加双丙酚丁

Determination of Oxyphenisatin Dipropionate in Weight Loss Compression Candies by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

郭跃平 叶欣彤 陈丽娥 董晓尉 黄秀彦
食品工业2024,Vol.45Issue(7) :306-309.

UPLC-MS/MS法测定减肥类压片糖果中非法添加双丙酚丁

Determination of Oxyphenisatin Dipropionate in Weight Loss Compression Candies by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

郭跃平 1叶欣彤 1陈丽娥 1董晓尉 1黄秀彦1
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作者信息

  • 1. 金华市食品药品检验检测研究院(金华 321000)
  • 折叠

摘要

建立快速、准确测定减肥类压片糖果中非法添加双丙酚丁的UPLC-MS/MS法.样品以80%甲醇水溶液为提取液,超声提取,采用Waters BEH-C18(2.1 mm×100mm,1.7 μm)色谱柱,以乙腈-5 mmol/L乙酸铵水溶液为流动相进行梯度洗脱,流速0.4 mL/min,进样量2 μL,柱温40 ℃,在正离子模式下电离,MRM模式检测,外标法定量.结果表明,双丙酚丁在1.0~100.0 ng/mL范围内线性关系良好,相关系数r为0.999 5,在加标浓度分别为0.05,1.0,5.0和10.0 mg/kg(n=6)时,回收率为87.6%~89.7%,SRSD为2.42%~2.61%,检出限为0.010 mg/kg,定量限为0.030 mg/kg.该方法简单快捷、精密度好、准确度高,适合大批量样品的测定,具有较强的实用价值.

Abstract

To establish an analysis method for the determination of oxyphenisatin dipropionate in weight loss compression candies by ultra performance liquid chromatography tandem mass spectrometry,the samples were extracted by 80%methanol water solution sonication.Then,waters BEH-C18(2.1 mm× 100 mm,1.7 μm)was adopted with the mobile phase of acetonitrile-ammonium acetate aqueous solution(5 mmol/L)in gradient elution.The flow rate was 0.4 mL/min,the sample volume was 2 μL,and the temperature of column was 40 ℃,thereafter,ionized in the positive ion mode,detected by multi-reaction monitoring and quantified by external standard.The results showed that the standard curves of oxyphenisatin dipropionate in the range of 0.05,1.0,5.0 and 10.0 mg/kg(n=6)showed good linearity,and the correlation coefficient r was 0.999 5.The average recoveries of oxyphenisatin dipropionate were 87.6%-89.7%in range of 0.05-10.0 mg/kg addition,and the relative standard deviation was 2.42%-2.61%.The detection limit and quantification limit were 0.010 mg/kg and 0.030 mg/kg,respectively.The method is simply,rapidly,highly accurate and accuracy,which is suitable for the determination of large quantities of samples with strong practical value.

关键词

UPLC-MS/MS法/减肥类压片糖果/双丙酚丁

Key words

UPLC-MS/MS/weight loss compression candies/oxyphenisatin dipropionate

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出版年

2024
食品工业
上海市食品工业研究所

食品工业

影响因子:0.47
ISSN:1004-471X
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