应用高效液相色谱与质谱联用建立了30种常见生物碱的质谱图与保留时间参数的数据库。分析时按以下条件进行:① 色谱柱:ZORBAX sb-aq.(2.1 mm×150 mm,3.5 μm,带预柱);② 柱温:30 ℃;③ 流动相:甲酸-水(0.1+99.9)混合溶液与甲酸-甲醇(0.1+99.9)混合溶液以不同比例混合后进行梯度淋洗;④ 流量:0.4 mL·min-1;⑤ 进样体积:10 μL;⑥ 用电喷雾离子化电离源;⑦ 自动3级质谱扫描;⑧ 扫描范围:50~1 000 aum。用谱图的解卷积和保留时间锁定软件,实现了药物中生物碱筛选的自动化操作。用所提出的方法替代常用方法对几件实际案件进行检验,结果表明:此方法具有避免漏检及降低假阳性报告机率的优点。

HPLC in hyphenation with MS was applied to establish data base of mass spectra and parameters of retention time of 30 common alkaloids. Analytical procedures were carried out under the following conditions: ① chromatographic column :ZORBAX sb-aq. (2.1 mm×150 mm, 3.5 μm, with precolumn); ② column temp.: 30 ℃; ③ mobile phase: mixture of formic acid+water (0.1+99.9) and formic acid+methanol (0.1+99.9) in different ratios for gradient elution; ④ flow-rate: 0.4 mL·min-1; ⑤ vol. of sample introduction: 10 μL; ⑥ electrospray ionization source (ESI); ⑦ automatic ternary MS scanning; ⑧ scanning range: 50-1 000 aum. Automation in operations of screening of alkaloids in drugs was attained by using the software of de-convolution of spectra and locking on retention times. The proposed method has been used instead of the conventional manual operations, in the inspection of substantial cases, displaying its specificity of avoiding missing in detection and decreasing the probability of false-positivity.