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0.2~0.5μg／kg和0.5~2.0μg／kg，加标回收率为79.5％~103.8％，RSD为3.6％~15.4％，在0.2~200.0μg／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。
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. Multi-ple technologies were applied to solve the identification and quantification for the two com-pounds,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 C 18 column was used to separate the analytes. The LODs and LOQs for BMPEA and picamilon in liquid,table and cap-sule samples were 0. 2-0. 5 μg/kg and 0. 5-2. 0 μg/kg,respectively. The average spiked recover-ies 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.
参考文献
| [1] | Cui, WQ;Chen, XY;Zhan, Y;Zhang, ZZ;Zhang, YF;Zhong, DF.Determination of picamilon concentration in human plasma by liquid chromatography-tandem mass spectrometry[J].Journal of chromatography, B. Analytical technologies in the biomedical and life sciences,201015/16(15/16):1181-1184. |
| [2] | Deventer, K.;Roels, K.;Delbeke, F.T.;Van Eenoo, P..Prevalence of legal and illegal stimulating agents in sports[J].Analytical and bioanalytical chemistry,20112(2):421-432. |
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