HPLC-DAD-MS/MS检测止咳平喘类中药制剂中非法添加的12种化学药品

建立止咳平喘类中药制剂中非法添加的12种化学药品的快速筛选方法.采用液相色谱-串联质谱法,以Kromasil 100-5C 18 (250 mm×4.6 mm,5μm)为分析柱,流动相采用0.3％甲酸铵(用甲酸调至pH 2.97)和甲醇进行梯度洗脱,电喷雾电离(ESI)、全扫描一级质谱和全扫描二级质谱扫描方式,对止咳平喘类中药制剂中非法添加的12种化学药品进行筛选分析.建立了快速分离、检测止咳平喘类中药制剂中非法添加的12种化学药品的方法,检测限低于50 ng.该方法专属性强、灵敏度高,适用于止咳平喘类中药制剂中非法添加化学药品的筛选及确证工作.

HPLC-DAD-MS/MS对栀子中色素成分的研究

目的 鉴定栀子中藏红花素类色素成分.方法 色谱条件:Dikma Diamonsil C18色谱柱(4.6 mm×250 mm,5μm)；0.15％甲酸水-甲醇梯度洗脱,流速0.6 mL/min,柱温30℃,检测波长440 nm.质谱条件:电喷雾离子源(ESI)；负离子模式检测；扫描范围m/z 100-1400.结合化学成分的紫外-可见吸收光谱特征,与多级质谱(MS/MS)裂解特征分析,对其结构进行确证.结果 采用高效液相色谱-二级管阵列检测器(HPLC-DAD)鉴别了栀子中的31个藏红花素类色素成分,并根据MS/MS裂解规律推断了其中的23个化学成分.结论 HPLC-DAD-MS/MS可用于快速筛选和鉴定栀子中的藏红花素类色素成分.

HPLC-DAD-MS/MS法结合谱库筛查5种中药中21种合成染料

目的 通过高效液相色谱-二极管阵列检测-串联质谱(HPLC-DAD-MS/MS)法结合谱库筛查龙血竭、红花、跌打丸、二十五味珊瑚丸、跌打活血散中21种合成染料(金胺O、金橙Ⅱ、胭脂红等).方法 7批阳性样品甲醇或乙醇提取液的分析采用Phenomenon Luna C18色谱柱(250 mm×4.6 mm,5μm);以乙腈-0.05 mol/L醋酸铵为流动相,梯度洗脱;体积流量1 mL/min;柱温40℃;检测波长400 ～ 700 nm.MS分析采用ESI电离源;干燥气温度350℃,体积流量10L/min;雾化气压力241.3 kPa;源电压4 kV.结果 所有样品均检测出合成染料,谱库匹配度均大于99.8.结论 该方法准确快速,可用于中药中合成染料筛查.

A quality control (QC) strategy for quantitative and qualitative analysis of “common peaks” in chemical fingerprint was proposed to analyze Yuanhu Zhitong tablet (YZT), using high performance liquid chromatography with diode array detector and tandem mass spectrometry (HPLC-DAD-MS/MS). The chromatographic separation was achieved on an Agilent Eclipse plus C18 column with a gradient elution using a mixture of 0.4‰ ammonium acetate aqueous (pH 6.0 adjusted with glacial acetic acid) and acetonitrile. In chemical fingerprint, 40 peaks were assigned as the “common peaks”. For quantification of “common peaks”, the detection wavelength was set at 254 nm, 270 nm, 280 nm and 345 nm, respectively. The method was validated and good results were obtained to simultaneously determine 10 analytes (protopine, jatrorrhizine, coptisine, palmatine, berberine, xanthotoxin, bergapten, tetrahydropalmatine, imperatorin and isoimperatorin). For qualification of “common peaks”, 33 compounds including 10 quantitative analytes were identified or tentatively characterized using LC-MS/MS. These results demonstrated that the present approach may be a powerful and useful tool to tackle the complex quality issue of YZT.