HPLC-QqQ-MS法同时测定八味小檗皮胶囊中25种成分的含量
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篇名: HPLC-QqQ-MS法同时测定八味小檗皮胶囊中25种成分的含量
TITLE: Simultaneous determination of 25 components in Bawei xiaobopi capsules by HPLC-QqQ-MS
摘要: 目的 建立同时测定八味小檗皮胶囊中小檗碱、木兰花碱、羟基红花黄色素A等25种成分含量的方法。方法采用高效液相色谱串联三重四极杆质谱(HPLC-QqQ-MS)法。以WondaSilC18-WR为色谱柱,以0.1%甲酸溶液-甲醇为流动相进行梯度洗脱,柱温为25℃,流速为0.5mL/min,进样量为5μL;采用电喷雾离子源,正、负离子模式下同时扫描,多重反应监测模式进行测定,毛细管电压分别为4000V(+)、2500V(-),干燥气流速为11L/min,温度为300℃,压力为15psi。结果八味小檗皮胶囊中木兰花碱、药根碱、小檗碱、巴马汀、蟾蜍色胺、蟾蜍特尼定、胡椒碱、甘草酸、阿魏酸、阿魏酸4-O-β-D-吡喃葡萄糖苷、羟基红花黄色素A、绿原酸、没食子酸、诃子鞣酸、柯里拉京、鞣花酸、甘草素、甘草苷、芦丁、槲皮素、甘氨胆酸、胆酸、甘氨鹅脱氧胆酸、甘氨脱氧胆酸、熊去氧胆酸在各自的质量浓度范围内线性关系良好(r≥0.9990);定量限为0.62~554.50ng/mL,检测限为0.18~166.30ng/mL;精密度、重复性、稳定性(24h)试验的RSD均小于3.00%;加样回收率均在80%~115%之间(RSD均小于3.00%,n=6)。上述25种成分的含量分别为16.94~20.82、3.78~5.17、9.11~11.43、0.24~0.30、0.20~0.39、0.74~1.16、0.79~0.89、3.26~3.35、0.48~0.66、11.96~13.35、2.30~3.12、0.19~0.21、6.07~8.83、10.42~10.48、1.43~1.64、4.17~4.76、0.14~0.15、0.46~0.52、0.04、0.01、0.59~0.63、0.20~0.23、0.02、0.15~0.16、0.01mg/g。结论所建立的含量测定方法简单、灵敏、稳定性好,可用于同时测定八味小檗皮胶囊中25种成分的含量。
ABSTRACT: OBJECTIVE To esta blish the method for simultaneous determination of 25 components (such as berberine , magnoflorine and hydroxysafflor yellow A )in Bawei xiaobopi capsules. METHODS High-performance liquid chromatography- tandem triple quadrupole mass spectrometry (HPLC-QqQ-MS)method was adopted. The determination was performed on WondaSil C18-WR column with mobile phase consisted of 0.1% formic acid solution-methanol (gradient elution )at the flow rate of 0.5 mL/min. The column temperature was 25 ℃,and sample size was 5 μL. Electrospray ionization source was scanned in positive and negative ion mode at the same time ,with multiple reaction monitoring. The capillary voltage was 4 000 V(+)and 2 500 V(-). The drying gas flow rate was 11 L/min with the temperature of 300 ℃. The pressure was 15 psi. RESULTS Totally 25 components of Bawei xiaobopi capsules had good linear relationship within a certain range ,such as magnolflorine ,jatrorrhizine,berberine, palmatine,bufotenine,bufotenidine,piperine,glycyrrhizic acid ,ferulic acid ,ferulic acid 4-O-β-D-glucopyranoside,hydroxysafflor yellow A ,chlorogenic acid ,gallic acid ,chebulagic acid ,corilagin,ellagic acid ,liquiritigenin,liquiritin,rutin,quercetin, glycocholic acid ,cholic acid ,glycochenodeoxycholic acid ,glycodeoxycholic acid ,ursodeoxycholic acid (r≥0.999 0). The limits of quantitation were 0.62-554.50 ng/mL;the limits of detection were 0.18-166.30 ng/mL.RSDs of precision ,repeatability and stability(24 h)tests were all lower than 3.00%. The recovery rates were 80%-115%(all RSDs lower than 3.00%,n=6). The contents of above 25 components were 16.94-20.82,3.78-5.17,9.11-11.43,0.24-0.30,0.20-0.39,0.74-1.16,0.79-0.89,3.26-3.35, 0.48-0.66,11.96-13.35,2.30-3.12,0.19-0.21,6.07-8.83,10.42-10.48,1.43-1.64,4.17-4.76,0.14-0.15,0.46-0.52,0.04,0.01, 0.59-0.63,0.20-0.23,0.02,0.15-0.16,0.01 mg/g,respectively. CONCLUSIONS Established method is simple ,sensitive and stable,and can be used for content determination of 25 components in Bawei xiaobopi capsules simultaneously.
期刊: 2022年第33卷第14期
作者: 易欢,彭芳,谢雨宸,苟晓玲,丁银,范刚
AUTHORS: YI Huan,PENG Fang,XIE Yuchen ,GOU Xiaoling ,DING Yin,FAN Gang
关键字: 藏药;八味小檗皮胶囊;含量测定;高效液相色谱串联三重四极杆质谱法
KEYWORDS: Tibetan medicine ;Bawei xiaobopi capsules ;
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