色谱 ›› 2016, Vol. 34 ›› Issue (7): 681-685.DOI: 10.3724/SP.J.1123.2016.03029

• 特别策划:出入境检验检疫系统专栏(2016) • 上一篇    下一篇

超高效液相色谱-多反应选择离子监测同步在线全扫描质谱技术测定保健品中的类安非他命和匹卡米隆

祝伟霞1, 张莉1, 李睢2, 张丽1, 刘亚风1, 杨冀州1   

  1. 1. 河南出入境检验检疫局, 河南 郑州 450003;
    2. 河南中医药大学, 河南 郑州 450000
  • 收稿日期:2016-03-22 出版日期:2016-07-08 发布日期:2013-02-05
  • 通讯作者: 杨冀州
  • 基金资助:

    国家质检总局科技计划项目(2015IK115);河南省科技攻关项目(122102110167,122102210393).

Determination of β-methylphenethylamine and picamilon in health products by ultra performance liquid chromatography-multiple reaction monitoring and online full scan mass spectrometry

ZHU Weixia1, ZHANG Li1, LI Sui2, ZHANG Li1, LIU Yafeng1, YANG Jizhou1   

  1. 1. Henan Entry-Exit Inspection and Quarantine Bureau, Zhengzhou 450003, China;
    2. Henan University of Chinese Medicine, Zhengzhou 450000, China
  • Received:2016-03-22 Online:2016-07-08 Published:2013-02-05
  • Supported by:

    General Administration of Quality Supervision, Inspection and Quarantine of the People's Scientific and Technological Projects (No. 2015IK115);Henan Province Key Scientific and Technological Projects (Nos. 122102110167, 122102210393).

摘要:

建立了超高效液相色谱-三重四极杆串联线性离子阱质谱测定保健品中类安非他命(BMPEA)和匹卡米隆的分析方法。样品采用甲醇超声提取,新型反相固相萃取柱(PRiME HLB)净化,采用甲醇-0.1%(v/v)甲酸水溶液作为流动相,SHISEIDO CAPCELL MG Ⅱ C18色谱柱分离BMPEA和匹卡米隆。在电喷雾离子源正离子电离模式下,联合采用多反应选择离子监测(MRM)、增强型子离子全扫描(EPI)和谱库检索技术,实现了两种分析物的定性分析和定量计算。在该实验条件下,BMPEA和匹卡米隆在口服液、片剂和胶囊样品中的检出限(LOD)和定量限(LOQ)分别为0.2~0.5 μg/kg和0.5~2.0 μg/kg,加标回收率为79.5%~103.8%, RSD为3.6%~15.4%,在0.2~200.0 μg/kg范围内基质标准溶液的含量和峰面积呈良好线性关系(r≥0.9969)。该方法成功应用于进口和市售保健品的测定,分析结果表明该方法操作简单、结果准确,可用于保健品中BMPEA和匹卡米隆的确证分析。

关键词: 保健品, 超高效液相色谱-三重四极杆线性离子阱质谱, 固相萃取, 类安非他命, 匹卡米隆, 增强型子离子全扫描

Abstract:

A confirmative method was developed for determining β-methylphenethylamine (BMPEA) and picamilon in health products by ultra performance liquid chromatography-triple quadrupole linear ion trap mass spectrometry (UPLC-Q Trap MS). The sample was ultrasonically extracted with methanol. The purification was carried out on a new reversed phase solid-phase extraction column (PRiME HLB). The detection of compounds was in the positive mode. Multiple technologies were applied to solve the identification and quantification for the two compounds, such as multiple reaction monitoring (MRM), online enhanced product ion full scan (EPI) and library search. Methanol and 0.1% (v/v) formic acid aqueous solution were used as the mobile phases with gradient elution. A SHISEIDO CAPCELL MG Ⅱ C18 column was used to separate the analytes. The LODs and LOQs for BMPEA and picamilon in liquid, table and capsule samples were 0. 2-0.5 μg/kg and 0.5-2.0 μg/kg, respectively. The average spiked recoveries of the method varied from 79.5% to 103.8% and the RSDs were between 3.6% and 15.4%. In the range of 0.2-200.0 μg/kg, the peak areas and concentrations of matrix standard solution showed good linear relationship (r≥0.9969). The qualitative confirmation results were required based on the search-match MRM and EPI mass spectra simultaneously. The method is simple and accurate for the determination of BMPEA and picamilon in imported and commercial health products.

Key words: β-methylphenethylamine (BMPEA), enhanced product ion full scan (EPI), health products, picamilon, solid-phase extraction (SPE), ultra performance liquid chromatography-triple quadrupole linear ion trap mass spectrometry (UPLC-Q Trap MS)

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