色谱

色谱 ›› 2019, Vol. 37 ›› Issue (12): 1331-1336.DOI: 10.3724/SP.J.1123.2019.05035

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法测定酵素食品中的匹可硫酸钠

何嘉雯, 温家欣, 赖宇红, 刘亚雄, 曹雅静, 陈俏   

  1. 广东省药品检验所, 广东 广州 510180
  • 收稿日期:2019-05-22 出版日期:2019-12-08 发布日期:2020-12-11
  • 通讯作者: 何嘉雯.E-mail:hjw7hjw@163.com.
  • 基金资助:
    广东省省级科技计划项目（2015A030401062）；国家市场监督管理总局项目.

Determination of sodium picosulfate in enzyme products by high-performance liquid chromatography-tandem mass spectrometry

HE Jiawen, WEN Jiaxin, LAI Yuhong, LIU Yaxiong, CAO Yajing, CHEN Qiao   

  1. Guangdong Institute for Drug Control, Guangzhou 510180, China
  • Received:2019-05-22 Online:2019-12-08 Published:2020-12-11
  • Supported by:
    Science and Technology Planning Project of Guangdong Province (No. 2015A030401062); Project of State Administration for Market Regulation.

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摘要： 建立了高效液相色谱-串联质谱法测定酵素食品中新型减肥类非法添加物匹可硫酸钠的分析方法。针对现有方法不适用的果冻、软糖型样品，开发了新的前处理方法。样品经水提取、聚酰胺净化，使用Thermo Accucore RP-MS色谱柱（100 mm×2.1 mm，2.6 μm），以乙腈-10 mmol/L乙酸铵（15：85，v/v）等度洗脱，流速0.3 mL/min，柱温35℃，多反应监测（MRM）模式下质谱检测，外标法定量。结果表明，匹可硫酸钠在5~500 μg/L范围内线性关系良好，相关系数（r）为0.9999，方法检出限为0.05 mg/kg。匹可硫酸钠在各基质样品中的加标回收率为89.2%~111.8%，相对标准偏差为2.5%~10.4%。按上述方法检测152批次酵素食品，检出阳性样品58批次，检出率为38.2%。该法准确、灵敏，可用于酵素食品中匹可硫酸钠的测定。

关键词: 高效液相色谱-串联质谱法, 匹可硫酸钠, 酵素食品, 非法添加, 减肥

Abstract: A method based on high-performance liquid chromatography-tandem mass spectrometry was developed for the determination of sodium picosulfate in enzyme products. Sodium picosulfate is a new slimming aid that is illegally added to food products. The existing analytical methods are not suitable for application to jellies and gel candies, thus triggering the need for developing a new method. The samples were extracted with water and passed through a polyamide cartridge. The extracts were separated on a Thermo Accucore RP-MS column (100 mm×2.1 mm, 2.6 μm) using acetonitrile-10 mmol/L ammonium acetate solution (15:85, v/v) as the mobile phase. The flow rate of the mobile phase was 0.3 mL/min, and the column temperature was 35 ℃. Detection was carried out in the multiple reaction monitoring (MRM) mode. Quantification analysis was performed by the external standard method. The results showed that sodium picosulfate had a good linear relationship in the range of 5-500 μg/L, and the correlation coefficient (r) was 0.9999. The limit of detection (LOD) was 0.05 mg/kg. The average recoveries of sodium picosulfate in different matrices were in the range of 89.2%-111.8%, with the relative standard deviations (RSDs) of 2.5%-10.4%. The method was applied to the analysis of 152 samples, and 58 positive samples were detected. The positive rate was 38.2%. The developed method is accurate and sensitive, and it is suitable for detecting sodium picosulfate in enzyme products.

Key words: high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), sodium picosulfate, enzyme product, illegally added, slimming

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