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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 ； |
| 阅读数： | 265 次 |
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