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-C_(18)(2.1 mm×100 mm, 1.7μm)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2μL,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10.0mg/kg (n=6)时,回收率为87.6%~89.7%, S_(RSD)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。
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-Cis(2.1 mmx100 mm,1.7μm)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 2μL,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 coeficient r was 0.9995.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.
作者
郭跃平
叶欣彤
陈丽娥
董晓尉
黄秀彦
GUO Yueping;YE Xintong;CHEN Li'e;DONG Xiaowei;HUANG Xiuyan(Insititute for Food and Drug Inspection and Testing of Jinhua,Jinhua 321000)
出处
《食品工业》
CAS
2024年第7期306-309,共4页
The Food Industry
