HPLC-ELSD法测定心脑苏滴丸中银杏内酯含量
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摘要
目的建立高效液相色谱-蒸发光散射检测(HPLC-ELSD)法测定心脑苏滴丸中的银杏内酯(白果内酯、银杏内酯A、银杏内酯B和银杏内酯C)的含量。方法采用十八烷基硅烷键合硅胶色谱柱(Thermo,Hypersil 250 mm×4.6 mm,5μm),以正丙醇-水(1∶84,V/V)混合液(A)和四氢呋喃(B)为流动相,柱温35℃,流动相流速1 mL·min~(-1),漂移管温度为50℃,气体流量为1.2 L·min~(-1)。结果 HPLC-ELSD法可同时测定的白果内酯、银杏内酯A、银杏内酯B和银杏内酯C,白果内酯在0.0434～0.136 mg·mL~(-1)浓度范围内,银杏内酯A在0.734～1.835 mg·mL~(-1)浓度范围内,银杏内酯B在0.366～0.915 mg·mL~(-1)浓度范围内,银杏内酯C在0.417～1.336 mg·mL~(-1)浓度范围内分别呈良好的线性关系。结论本方法灵敏度高,准确性强,适用于测定心脑苏滴丸中的白果内酯、银杏内酯A、银杏内酯B和银杏内酯C含量。
OBJECTIVE To establish the method to determine the content of ginkgolides( bilobalide,ginkgolide A,ginkgolide B and ginkgolide C) in Xinnaosu dropping pills by HPLC-ELSD. METHODS A HPLC-ELSD method was set. Thermo C18( 250 mm×4.6 mm,5 μm) was used.The Normal propyl alcohol was mixed with water in 1 ∶84 as mobile phase A and tetrahydrofuran as mobile phase B.The column temperature was set at 35 ℃.The flow rate was 1.0 m L·min~(-1).The tube temperature of the detertor was 50 ℃.The gain flow rate was 1.2 L·min~(-1). RESULTS The bilobalide,ginkgolide A,ginkgolide B and ginkgolide C were determined by HPLC-ELSD. The bilobalide,ginkgolide A,ginkgolide B and ginkgolide C were linear at the range of 0.0434-0.136 mg·mL~(-1),0.734~(-1).835 mg·mL~(-1),0.366-0.915 mg·mL~(-1) and 0.417~(-1).336 mg·mL~(-1) respectively. The average recovery were from 95% to 105%. CONCLUSION This method is sensitive and accurate for the determination of bilobalide,ginkgolide A,ginkgolide B and ginkgolide C in Xinnaosu dropping pills.
OBJECTIVE To establish the method to determine the content of ginkgolides( bilobalide,ginkgolide A,ginkgolide B and ginkgolide C) in Xinnaosu dropping pills by HPLC-ELSD. METHODS A HPLC-ELSD method was set. Thermo C18( 250 mm×4.6 mm,5 μm) was used.The Normal propyl alcohol was mixed with water in 1 ∶84 as mobile phase A and tetrahydrofuran as mobile phase B.The column temperature was set at 35 ℃.The flow rate was 1.0 m L·min~(-1).The tube temperature of the detertor was 50 ℃.The gain flow rate was 1.2 L·min~(-1). RESULTS The bilobalide,ginkgolide A,ginkgolide B and ginkgolide C were determined by HPLC-ELSD. The bilobalide,ginkgolide A,ginkgolide B and ginkgolide C were linear at the range of 0.0434-0.136 mg·mL~(-1),0.734~(-1).835 mg·mL~(-1),0.366-0.915 mg·mL~(-1) and 0.417~(-1).336 mg·mL~(-1) respectively. The average recovery were from 95% to 105%. CONCLUSION This method is sensitive and accurate for the determination of bilobalide,ginkgolide A,ginkgolide B and ginkgolide C in Xinnaosu dropping pills.
引文
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[7]秦建平,吴建雄,潘有智,等. HPLC-ELSD法测定白果中银杏内酯A、银杏内酯B和银杏内酯C[J].现代药物与临床,2016,31(2):155-157.
[8]曹邦静,苏娟,叶霖,等.蒸发光散射检测器在中药分析中的应用[J].药学实践杂志,2015,33(1):13-14.
[9]廖小芳,毕晓黎,胥爱丽,等.市售不同产地黄芪HPLC-DADELSD指纹图谱及同时测定3种成分含量的方法研究[J].广东药科大学学报,2018,34(5):558-563.
[10]来李娟,崔田,邓祖磊,等.HPLC-ELSD法测定灵芝中灵芝酸A的含量[J].广东药科大学学报,2017,33(5):617-619.
[2]Lv P,Fang W,Geng X,et al. Therapeutic neuroprotective effects of ginkgolide B on cortex and basal ganglia in a rat model of transient focal ischemia[J]. Eur J Parm Sci,2011,44(3):235-240.
[3]王旋,顾振纶,秦振红,等.银杏内酯A和B混合物对大鼠永久性局灶性脑缺血的保护作用[J].中草药,2007,38(2):241-244.
[4]胡清文,任冬梅,杨爽.银杏内酯和银杏叶胶囊对大鼠脑缺血治疗的对比研究[J].中药材,2012,35(3):449-451.
[5]任俊,贾正平,邓虹珠,等.银杏内酯对三种脑缺血模型大鼠的保护作用[J].中药新药与临床药理,2005,169(1):41-45.
[6]高蓓. HPLC-ELSD法测定银杏滴丸中银杏内酯A、B、C和白果内酯[J].中草药,2010,41(2):236-238.
[7]秦建平,吴建雄,潘有智,等. HPLC-ELSD法测定白果中银杏内酯A、银杏内酯B和银杏内酯C[J].现代药物与临床,2016,31(2):155-157.
[8]曹邦静,苏娟,叶霖,等.蒸发光散射检测器在中药分析中的应用[J].药学实践杂志,2015,33(1):13-14.
[9]廖小芳,毕晓黎,胥爱丽,等.市售不同产地黄芪HPLC-DADELSD指纹图谱及同时测定3种成分含量的方法研究[J].广东药科大学学报,2018,34(5):558-563.
[10]来李娟,崔田,邓祖磊,等.HPLC-ELSD法测定灵芝中灵芝酸A的含量[J].广东药科大学学报,2017,33(5):617-619.