气相色谱法测定辽藁本中藁本内酯、正丁基苯酞含量
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摘要
目的:建立气相色谱测定方法,同时测定辽藁本中藁本内酯、正丁基苯酞含量,为辽藁本制定质量标准提供依据。方法:采用气相色谱法,HP-5MS气相色谱柱、分流不分流进样口、FID检测器。进样口温度:250℃,检测器:温度300℃,H_2:40 m L·min~(-1),空气:400 m L·min~(-1),流速1m L·min~(-1),程序升温条件:50℃,10℃·min~(-1)至94℃,2℃·min~(-1)至102℃,5℃·min~(-1)至130℃,2℃·min~(-1)至144℃,0.5℃·min~(-1)至145.5℃,0.2℃·min~(-1)至146.8℃,后运行5分钟至280℃。结果:建立辽藁本中藁本内酯、正丁基苯酞含量测定方法。藁本内酯、正丁基苯酞线性范围分别为:85.6~684.8μg·ml~(-1)、46.13~738μg·ml~(-1)。精密度、重复性、8 h稳定性、加样回收率良好。结论:该方法操作简便,结果准确,可用于辽藁本中藁本内酯、正丁基苯酞含量测定。
Objective: Establish GC method to determine Ligustilide and N-butyl phthalide contents. Provide the basis for quality standards of Ligusticum jeholense. Method: Use gas chromatography,HP-5 MS gas chromatography column,split/splitless inlet temperature: 250 ℃,FID detecter: 300 ℃,H_2: 40 m L·min~(-1),atmosphere: 400 m L·min~(-1),flow rate: 1 m L·min~(-1),temperatuer program condition: 50 ℃,10 ℃ ·min~(-1) to 94 ℃,2℃ ·min~(-1) to 102 ℃,5 ℃ ·min~(-1) to130 ℃,2 ℃ ·min~(-1) to 144 ℃,0. 5 ℃ ·min~(-1) to 145 ℃,0. 2 ℃ ·min~(-1) to 146. 8 ℃,post run 5 min to 280℃. Result:Established the method of determine Ligustilide and N-butyl phthalide in Ligusticum jeholense by GC. The linear ranges were: 85. 6 ~ 684. 8μg·ml~(-1)、46. 13 ~ 738μg·ml~(-1). This method has good precision,repeatability,stability of 8 hours and recovery. Conclusion: This method is simple,accurate and can be used for quality control of Ligustilide and N-butyl phthalide in Ligusticum jeholense.
Objective: Establish GC method to determine Ligustilide and N-butyl phthalide contents. Provide the basis for quality standards of Ligusticum jeholense. Method: Use gas chromatography,HP-5 MS gas chromatography column,split/splitless inlet temperature: 250 ℃,FID detecter: 300 ℃,H_2: 40 m L·min~(-1),atmosphere: 400 m L·min~(-1),flow rate: 1 m L·min~(-1),temperatuer program condition: 50 ℃,10 ℃ ·min~(-1) to 94 ℃,2℃ ·min~(-1) to 102 ℃,5 ℃ ·min~(-1) to130 ℃,2 ℃ ·min~(-1) to 144 ℃,0. 5 ℃ ·min~(-1) to 145 ℃,0. 2 ℃ ·min~(-1) to 146. 8 ℃,post run 5 min to 280℃. Result:Established the method of determine Ligustilide and N-butyl phthalide in Ligusticum jeholense by GC. The linear ranges were: 85. 6 ~ 684. 8μg·ml~(-1)、46. 13 ~ 738μg·ml~(-1). This method has good precision,repeatability,stability of 8 hours and recovery. Conclusion: This method is simple,accurate and can be used for quality control of Ligustilide and N-butyl phthalide in Ligusticum jeholense.
引文
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[2]林乔,赵爱国,陈建南,等.藁本内酯镇痛抗炎作用[J].中国实验方剂学杂志,2011,17(11):165-168.
[3]毛晓娜,杜俊蓉,旷喜,等.PPARγ激动剂藁本内酯的中枢抗炎作用及机制研究[J].中药药理与临床,2017,33(1):26-30.
[4]刘晓娇,周红静,杜俊蓉.藁本内酯对脂多糖诱导神经炎症的抑制作用[J].华西药学杂志,2016,31(4):353-356.
[5]杜旌畅,谢晓芳,熊亮,等.藁本内酯预处理对糖氧剥夺-复糖氧损伤血管内皮细胞火星及NO/NOS与HIF-1α、VEGF、Tubulin表达的影响[J].中药药理与临床,2016,32(5):31-35.
[6]Xu H L,Feng Y P.Inhibitory efects of chiral 3-n-buTylphthalide on inflammation following focal ischemic brain injuryin rats[J].Acta pharmacologica sinica,2000,21(5):433.
[7]种兆忠,冯亦璞.丁基苯酞对大脑中动脉阻断后皮层组织中花生四烯酸释放及磷脂酶A基因表达的影响[J].药学学报,2000,35(8):561-563.
[8]周毅,牛莉静,齐凤苗,等.丁基苯酞预处理对大鼠脑组织缺血/再灌注后HSP70表达的影响[J].中国应用生理学杂志,2015,31(2):136-140.
[9]支楠,徐群.丁基苯酞对脂多糖活化的小胶质细胞炎症介质释放的影响[J].上海交通大学学报,2016,36(12):1719-1722.
[10]张聪.正丁基苯酞对脑梗死后神经功能恢复作用的机制研究[D].石家庄:河北医科大学,2015.
[11]张爱君.藁本内酯对照品提取与稳定性研究[J].辽宁中医药大学学报,2008,10(5):162-163.