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

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。

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

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.