色谱 ›› 2019, Vol. 37 ›› Issue (2): 183-188.DOI: 10.3724/SP.J.1123.2018.10015

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时测定保健食品中丙磺舒、别嘌醇和苯溴马隆

邓幸飞1,2, 綦艳1, 李锦清1, 张燕1, 熊波1, 刘辉1   

  1. 1. 广东产品质量监督检验研究院, 国家食品质量监督检验中心(广东), 广东 佛山 528300;
    2. 华南农业大学, 广东 广州 510642
  • 收稿日期:2018-10-15 出版日期:2019-02-09 发布日期:2014-12-31
  • 通讯作者: 刘辉,E-mail:329520539@qq.com
  • 基金资助:

    广东省省级科技计划项目(2013B090600059).

Simultaneous determination of allopurinol, probenecid, benzbromarone in dietary supplements by ultra high performance liquid chromatography-tandem mass spectrometry

DENG Xingfei1,2, QI Yan1, LI Jinqing1, ZHANG Yan1, XIONG Bo1, LIU Hui1   

  1. 1. Guangdong Testing Institute of Product Quality Supervision, China National Quality Supervision and Testing Center for Food(Guangdong), Foshan 528300, China;
    2. South China Agricultural University, Guangzhou 510642, China
  • Received:2018-10-15 Online:2019-02-09 Published:2014-12-31
  • Supported by:

    Provincial Science and Technology Program in Guangdong Province (No. 2013B090600059).

摘要:

建立了基于QuEChERS前处理的超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定抗痛风类保健食品中别嘌醇、丙磺舒和苯溴马隆3种药物的检测方法。样品经含0.1%(v/v)氨水的乙腈溶液超声提取后,采用乙二胺-N-丙基硅烷(PSA)和十八烷基键合硅胶(C18)吸附剂净化,用C18色谱柱进行分离,0.1%(v/v)甲酸水溶液和甲醇为流动相进行梯度洗脱,采用电喷雾电离源、正负离子切换模式和多反应监测(MRM)模式检测。结果表明,别嘌醇、丙磺舒和苯溴马隆的检出限分别为5、25和25 μg/kg,定量限分别为17、80和80 μg/kg。抗痛风类保健食品中3种药物的平均加标回收率为76.8%~116.6%,相对标准偏差(RSD)为2.7%~14.6%。应用该法对68批次保健食品进行分析,其中1批次样品检出别嘌醇药物。该法操作简单,灵敏度高,可用于抗痛风类保健食品中别嘌醇、丙磺舒和苯溴马隆的测定。

关键词: QuEChERS, 保健食品, 苯溴马隆, 别嘌醇, 丙磺舒, 超高效液相色谱-串联质谱

Abstract:

A method based on QuEChERS purification was developed for the simultaneous determination of allopurinol, probenecid and benzbromarone in anti-gout dietary supplements by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted by acetonitrile mixed with 0.1% (v/v) ammonium hydroxide, and the extracts were purified using primary secondary amine (PSA) and C18 adsorbents. The samples were separated on a C18 chromatographic column with the gradient elution of 0.1% (v/v) formic acid aqueous solution and methanol as mobile phases. The analytes were detected by a electrospray ionization source in the positive or negative ion mode and the multiple reaction monitoring mode. The results showed that the limits of detection of allopurinol, probenecid and benzbromarone were 5, 25 and 25 μg/kg, and the limits of quantification were 17, 80 and 80 μg/kg. The average spiked recoveries of the three chemical drugs in dietary supplements were in the range of 76.8%-116.6% with the relative standard deviations of 2.7%-14.6%. The proposed method was applied for the analysis of 68 dietary supplements, and allopurinol was detected in one of them. This method is simple and sensitive, and can be used for the determination of the allopurinol, probenecid and benzbromarone in anti-gout dietary supplements.

Key words: allopurinol, benzbromarone, dietary supplements, probenecid, QuEChERS, ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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