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作 者:潘有智[1] 秦建平[1] 王宪平[1] 李家春[1] 黄文哲[1] 王振中[1] 萧伟[1]
机构地区:[1]江苏康缘药业股份有限公司(中药制药过程新技术国家重点实验室),连云港222001
出 处:《药学与临床研究》2016年第4期281-283,共3页Pharmaceutical and Clinical Research
基 金:国家"重大新药创制"--现代中药创新集群与数字制药技术平台(2013ZX09402203)
摘 要:目的:采用液相与四极杆飞行时间串联质谱(UPLC-QTOF-MS/MS)对指纹图谱中色谱峰进行研究,对痛安注射液中的生物碱类化学成分进行定性鉴别。方法:采用Agilent SBC18RRHD(3 mm×100 mm,1.8μm)色谱柱,以乙腈-0.1%甲酸为流动相进行梯度洗脱,流速0.4 m L·min-1,柱温为25℃,进样量为2μL。检测质谱采用电喷雾离子源(ESI)的飞行时间质谱,正离子模式下采集数据,一级质谱质荷比扫描范围m/z 100~1500,二级质谱质荷比扫描范围m/z30~500。结果:痛安注射液的指纹图谱色谱峰中共鉴别出12个成分。结论:本方法快速、准确地鉴定了痛安注射液的指纹图谱中的主要成分,为痛安注射液质量标准的完善提供依据。Objective: To identify the alkaloids of Tong'an injection fingerprint using ultra-performanceliquid chromatography with quadrupole- time-of-flight mass spectrometry (UPLC- QTOF-MS). Methods: TheUPLC was conducted with an Agilent SB- C18 RRHD column (3mmx 100 mm, 1.8 ^ m) and a gradient solventsystem consisting of acetonitrile (A)-0.1% formic acid (adding ammonium acetate 10 mmol per 1000 mL).The flow rate was 0.4m L-min_1, the column temperature was maintained at 25 ^ , the injection volume was2 ^ L . QTOF-MS and electrospray ion (ESI) source were applied for the qualitative analysis under the positiveion mode, with the MS full mass scan ranged from 100 m/z to 1500 mJz and the MS2 full mass scanranged from 30 m/z to 500 m/z. Results: Twelve major components of fingerprint chromatography were identified.Conclusion: The method established is simple and rapid in components analysis of fingerprint.The study can provide useful information for the perfection of quality standard of Tong'an Injection.
关 键 词:痛安注射液 UPLC-Q-TOF MS/MS 指纹图谱 化学成分
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