摘要
目的采用UPLC-QqQ-MS技术分析黄柏Phellodendron chinense Schneid生品、不同炒制程度盐炙品中黄柏碱、木兰花碱、药根红碱、药根碱、巴马红汀、小檗红碱、巴马汀、小檗碱、黄柏内酯、黄柏酮10种成分量的变化。方法将生黄柏在130~140、150~160、170~180℃下分别炒制3、4、5、6、7 min制得盐黄柏,采用ACQUITY UPLC BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm);流动相0.1%甲酸乙腈-0.1%甲酸水,梯度洗脱;体积流量0.25 mL/min;柱温35℃。采用电喷雾离子源(ESI源),正离子扫描模式;离子扫描范围m/z 50~1000;毛细管电离电压3.5 kV;源温度150℃;脱溶剂温度250℃;脱溶剂气体体积流量800 L/h;锥孔气体体积流量50 L/h;多反应监测模式(MRM)。结果10种成分在各自范围内线性关系良好,平均加样回收率96.79%~102.23%,RSD 0.01%~0.79%。黄柏盐炙过程中小檗碱、巴马汀、药根碱、黄柏碱、木兰花碱、黄柏内酯含量整体呈下降趋势;黄柏酮在170~180℃、炒制4 min时含量较高;小檗红碱、巴马红汀、药根红碱含量整体呈上升趋势;10种成分的变化尤以180℃炒制时含量变化最为明显。结论该方法准确、灵敏、高效,可用于黄柏的质量控制;不同的炒制温度及炒制时间对其10种成分的含量影响较大。
AIM Using UPLC-QqQ-MS technology to analyze the quantitative changes of ten constituents,phellodendrine,magnoflorine,jatrorrhzrubine,jatrorrhizine,palmatrubine,berberrubine,palmatine,berberine,obaculactone and obacunone in raw Phellodendron chinense Schneid and different salt-water processed products.METHODS P.chinense exposed to an environment of 130-140℃,150-160℃and 170-180℃for 3,4,5,6 and 7 min,respectively,were prepared into the different salt-water processed products.The analysis of samples was performed on a 35℃thermostatic ACQUITY UPLC BEH C_(18)column(2.1 mm×100 mm,1.7μm),with the mobile phase comprising of 0.1%formic acid acetonitrile-0.1%formic acid flowing at 0.25 mL/min in a gradient elution manner.Electrospray ion source(ESI source),positive ion scan mode was applied;ion scan range of m/z 50~1000;capillary ionization voltage of 3.5 kV;source temperature of 150℃;desolventizing temperature of 250℃;desolventizing gas flow rate of 800 L/h;cone gas volume flow of 50 L/h;and multiple reaction monitoring mode(MRM).RESULTS Ten constituents showed good linear relationships within their own ranges(r>0.9990),whose average recoveries were 96.79%-102.23%,with the RSDs of 0.01%-0.79%.During the processing,the salt-water products of P.chinense were found with a trend of decline in the content of berberine,palmatine,jatrorrhizine,phellodendrine,magnoflorine,and obaculactone;an overall upward trend in the content of berberrubine,palmatrubine,and jatrorrhizrubine;higher obacunone content frying at 170-180℃for 4 min;and especially obvious changes in the 10 constituents content frying at 180℃.CONCLUSION Given different frying temperature and time,this accurate,sensitive and efficient method produces a great change in the content of 10 constituents,and thus can be used for the quality control of P.chinense.
作者
李丽
张超
郑威
于颖琦
张凡
高慧
LI Li;ZHANG Chao;ZHENG Wei;YU Ying-qi;ZHANG Fan;GAO Hui(School of Pharmacy,Liaoning University of Traditional Chinese Medicine,Dalian 116600,China)
出处
《中成药》
CAS
CSCD
北大核心
2021年第11期3082-3088,共7页
Chinese Traditional Patent Medicine
基金
国家自然基金项目(81903801)
辽宁省自然基金项目(20180550942)
辽宁中医药大学大学生创新创业项目(201910162044)。
关键词
黄柏
化学成分
盐炙
UPLC-QqQ-MS
Phellodendron chinense Schneid
chemical constituents
saltwater-processing
UPLC-QqQ-MS
