LC-MS同时测定伤科黄水中8种成分的含量
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摘要
目的:采用LC-MS技术同时测定伤科黄水中8种有效成分的含量。方法:采用XBridge C_(18)色谱柱(2.10mm×100.00mm,2.50μm);柱温35℃;流动相A为水-甲酸(100∶0.3),流动相B为甲醇-甲酸(100∶0.3),梯度洗脱,0~15min 70%A,15~20min 70%~60%A,20~25min 60%~85%A;流速0.30mL/min。结果:黄柏碱、药根碱、表小檗碱、黄连碱、巴马汀、小檗碱、栀子苷、绿原酸8种成分在各检测条件下无明显干扰峰;在测定浓度范围内(1.00~1 000.00ng/mL)线性关系良好,相关系数R~2>0.9990;加样回收率均在95.00%~115.00%之间,RSD均<5.00%;精密度RSD均<5.00%。3个不同批次供试品的测定结果较一致。结论:本研究建立的LC-MS分析方法可用于同时测定伤科黄水中8种有效成分的含量。
Objective: The content of 8 active ingredients in the Shangke Huangshui was simultaneously determined by LC-MS technique. Methods: XBridge C_(18) column(2.10 mm×100.00 mm, 2.50μm) was applied: column temperature 35°C; mobile phase A was water-formic acid(100∶0.3), mobile phase B was methanol-formic acid(100∶0.3), gradient elution, 0 to 15 min, 70%A; 15 to 20 min, 70% to 60%A; 20 to 25 minutes, 60% to 85%A; flow rate was 0.30 mL/min. Results: There were 8 components, such as phellodendron, jatrorrhizine, epiberberine, coptisine, palmatine, berberine, geniposide and chlorogenic acid. There were no obvious interference peaks under various detection conditions. The linear relationship was good in the concentration range(1.00~1 000.00 ng/mL), the correlation coefficient R~2>0.9990; the recovery rate of the sample was between 95.00% and 115.00%, RSD<5.00%; precision RSD<5.00%. The results of three different batches of test samples were consistent. Conclusion: The LC-MS method established in this study can be used to simultaneously determine the content of 8 active ingredients in the Shangke Huangshui.
Objective: The content of 8 active ingredients in the Shangke Huangshui was simultaneously determined by LC-MS technique. Methods: XBridge C_(18) column(2.10 mm×100.00 mm, 2.50μm) was applied: column temperature 35°C; mobile phase A was water-formic acid(100∶0.3), mobile phase B was methanol-formic acid(100∶0.3), gradient elution, 0 to 15 min, 70%A; 15 to 20 min, 70% to 60%A; 20 to 25 minutes, 60% to 85%A; flow rate was 0.30 mL/min. Results: There were 8 components, such as phellodendron, jatrorrhizine, epiberberine, coptisine, palmatine, berberine, geniposide and chlorogenic acid. There were no obvious interference peaks under various detection conditions. The linear relationship was good in the concentration range(1.00~1 000.00 ng/mL), the correlation coefficient R~2>0.9990; the recovery rate of the sample was between 95.00% and 115.00%, RSD<5.00%; precision RSD<5.00%. The results of three different batches of test samples were consistent. Conclusion: The LC-MS method established in this study can be used to simultaneously determine the content of 8 active ingredients in the Shangke Huangshui.
引文
[1]蔡薇,廖锡锵.伤科黄水消除胫腓骨双骨折术前肿胀疗效观察.亚太传统医药,2017,13(2):140-141
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[7]高茹,林以宁,梁鸽,等.HPLC-DAD法同时测定茵黄合剂中绿原酸、栀子苷、黄芩苷和大黄酸的含量.中华中医药杂志,2017,32(3):1344-1347
[8]霍志鹏,王玉,周水平,等.黄连生物碱成分的HPLC-DAD-MS分析.天津药学,2016,28(2):8-12
[9]赵妍,张梅,任爱农,等.LC-MS/MS分析大鼠口服清清颗粒后血浆中9种成分的药代动力学.中国实验方剂学杂志,2017,23(1):85-90
[2]潘海文,王朝辉,李卓伟,等.伤科黄水预防断指再植术后血管危象的临床观察.中成药,2017,39(5):916-921
[3]罗学辉,谢学文,曾文磊,等.关节镜下有限清理术配合伤科黄水外敷治疗膝骨性关节炎的效果.广东医学,2016,37(7):1078-1081
[4]张建锋,刘文,侯晓杰,等.黄连超高液相色谱-质谱联用血清药物化学研究.时珍国医国药,2017,28(2):284-285
[5]孙振刚,邱昆成,李丹,等.UPLC-LTQ-Orbitrap XL分析知母-黄柏药对化学成分.中药材,2017,40(1):101-106
[6]徐姣,赵嵘,代云桃,等.栀子标准汤剂的质量评价方法考察.中国实验方剂学杂志,2017,23(7):30-35
[7]高茹,林以宁,梁鸽,等.HPLC-DAD法同时测定茵黄合剂中绿原酸、栀子苷、黄芩苷和大黄酸的含量.中华中医药杂志,2017,32(3):1344-1347
[8]霍志鹏,王玉,周水平,等.黄连生物碱成分的HPLC-DAD-MS分析.天津药学,2016,28(2):8-12
[9]赵妍,张梅,任爱农,等.LC-MS/MS分析大鼠口服清清颗粒后血浆中9种成分的药代动力学.中国实验方剂学杂志,2017,23(1):85-90