HPLC-MS/MS法鉴定半枝莲指纹图谱共有峰  

Identification of common peaks of herb Scutellaria barbata by HPLC-MS/MS

作　　者：王慧彬[1] 李琳[1] 张秀芝[1] 王英锋[2] 

机构地区：[1]北京市朝阳区疾病预防控制中心,北京100021 [2]首都师范大学,北京100037

出　　处：《中国卫生检验杂志》2015年第12期1922-1925,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的在已确定的半枝莲HPLC指纹图谱的基础上,用高效液相色谱/四极杆-飞行时间质谱(HPLC/Q-TOF-MS)联用技术,对其13个共有峰进行鉴定。方法采用Discovery-C18色谱柱(4.6 mm×250 mm,5μm),以甲醇-水(0.05%甲酸)的溶液进行梯度洗脱[时间:0 min→30 min→70 min,甲醇和水(0.05%甲酸)的体积比:25∶75→40∶60→75∶25],流速为1 ml/min,检测波长为335 nm,柱前分流,进样量为10μl,柱温为24℃,采用电喷雾正离子模式。结果对半枝莲药材的指纹图谱13个共有峰运用HPLC-MS/MS进行指认,基本确定每个峰的成分。结论基本鉴定了13个共有峰中10个峰可能的成分,1个峰单一用质谱的方法还不能确定,2个峰为半枝莲未见报道的成分。Objective Thirteen common peaks of Scutellaria barbata were identified by high performance liquid chromatography / quadrupole- time- of- flight mass spectrometry（ HPLC / Q- TOF / MS） on the basis of fingerprint of Scutellaria barbata which had been confirmed by HPLC. Methods The analytical column was Discovery- C18column（ 4. 6 mm × 250 mm,5 μm）; the mobile phase was composed of CH3 OH and H2O（ 0. 05% CHOOH） with a liner gradient elution [time： 0 min→30 min→70 min; elute rate of CH3 OH and H2O（ 0. 05% CHOOH） was 25∶75→40∶60→75∶25]. Flow rate was 1 ml / min;UV detection wave length was set at 335 nm; 10 μl sample was injected and the the column temperature was maintained at24 ℃. The mass spectrometer was operated under the positive ion mode with the ESI soure. Results Fingerprints of Scutellaria barbata with thirteen common peaks were identified by HPLC- MS / MS. The method could determine the components of each peaks basically. Conclusion Ten components of thirteen common peaks were identified. One peak of them could not be identified by mass spectrometry methods. The other two peaks showed the components not been reported in the study of Scutellaria barbata.

关 键 词：半枝莲 指纹图谱 高效液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学]