液相色谱-质谱法自动筛选常见30种生物碱  

Automatic Screening of 30 Alkaloids by Hyphenation of HPLC with MS

作　　者：王学虎[1] 袁敏[2] 张前上[1] 赵武生[1] 顾月保[1] 

机构地区：[1]江苏省公安厅物证鉴定中心,南京210024 [2]江苏出入境检验检疫局,南京210001

出　　处：《理化检验（化学分册）》2011年第4期427-429,432,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：江苏省公安厅科技处科研项目(200801001)

摘　　要：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.(2.1mm×150mm,3.5μm,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:0.4mL·min^(-1);⑤进样体积:10μL;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:50～1000aum。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：①chromatographic column：ZORBAX sb-aq.（2.1mm×150 mm,3.5μm,with precolumn）;②column temp.： 30℃;③mobile phase：mixture of formic acid ＋water（0.1＋99.9）and formic acid＋methanol（0.1＋99.9）in different ratios for gradient elution;④flow-rate：0.4mL·min^-1;⑤vol,of sample introduction;10μL;⑥electrospray ionization source（ESI）;⑦automatic ternary MS scanning;⑧scanning range：50-1000 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.

关 键 词：高效液相色谱-质谱联用 质谱库 自动筛选 解卷积 锁定保留时间 生物碱 

分 类 号：O657.63[理学—分析化学]