HPLC-CAD法同时测定元胡止痛胶囊中6种生物碱及香豆素类成分的含量
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摘要
目的建立HPLC-CAD法同时测定元胡止痛胶囊中延胡索乙素、黄藤素、去氢延胡索甲素、延胡索甲素、欧前胡素及异欧前胡素的含量,为元胡止痛胶囊的质量控制提供参考。方法采用高效液相色谱法联合电雾式检测器(HPLC-CAD法),色谱柱为Diamonsil C_(18)(250 mm×4.6 mm,5μm),乙腈(A)-0.05%甲酸铵(甲酸调pH至4.0)(B)为流动相,梯度洗脱(0~10 min,15%A;10~25 min,15%~30%A;25~40 min,30%~40%A;40~50 min,40%~70%A),柱温35℃,雾化器温度35℃,体积流量0.8 mL·min~(-1),进样量20μL,测定元胡止痛胶囊中6种生物碱及香豆素类成分的含量。结果延胡索乙素、黄藤素、去氢延胡索甲素、延胡索甲素、欧前胡素及异欧前胡素的质量浓度分别在0.040~1.010μg(r=0.9991)、0.013~0.320μg(r=0.9994)、0.068~1.700μg(r=0.9994)、0.041~1.020μg(r=0.9997)、0.101~2.520μg(r=0.9991)、0.039~0.980μg(r=0.9993)内与峰面积呈良好的线性关系。延胡索乙素、黄藤素、去氢延胡索甲素、延胡索甲素、欧前胡素及异欧前胡素的平均加样回收率分别为98.5%、98.9%、98.3%、99.4%、98.1%和98.7%,RSD(n=6)分别为0.90%、1.4%、0.70%、1.1%、0.70%和0.90%。结论该方法准确、简便、灵敏度高,可用于元胡止痛胶囊中生物碱和香豆素类多成分的质量控制研究。
Objective To develop an HPLC-CAD method to simultaneously determine 6 alkaloids and coumarins of dl-tetrahydropalmatine, palmatine, dehydrocorydaline, d-corydaline, imperatorin, and isoimperation in Yuanhu Zhitong capsules, and provide references for its quality control. Methods HPLC-CAD was used, chromatographic separation was performed on a Diamonsil C_(18) column(250 mm×4.6 mm, 5 μm). Acetonitrile(A)-0.05% ammonium acetate(acetic acid tone pH4.0)(B) was used as the mobile phase for gradient elution(0-10 min, 15% A; 10-25 min, 15%-30% A; 25-40 min, 30%-40% A; 40-50 min, 40%-70% A), the column temperature was maintained at 35 ℃, the nebulization temperature of detector was 35℃, the flow rate was 0.8 mL·min~(-1), and injection volume was 20 μL. The 6 components of Yuanhu Zhitong capsules were determined. Results The 6 components were linearity at 0.040-1.010 μg(r = 0.9991), 0.013-0.320 μg(r= 0.9994), 0.068-1.700 μg(r = 0.9994), 0.041-1.020 μg(r = 0.9997), 0.101-2.520 μg(r = 0.9991) and 0.039-0.980 μg(r = 0.9993), respectively. The average recoveries were 98.5%, 98.9%, 98.3%, 99.4%, 98.1% and 98.7%, and the RSDs were 0.90%, 1.4%, 0.70%, 1.1%, 0.70% and 0.90%. Conclusion The method is accurate, convenient and sensitive for the quality control of multicomponent of alkaloids and coumarins in Yuanhu Zhitong capsules.
Objective To develop an HPLC-CAD method to simultaneously determine 6 alkaloids and coumarins of dl-tetrahydropalmatine, palmatine, dehydrocorydaline, d-corydaline, imperatorin, and isoimperation in Yuanhu Zhitong capsules, and provide references for its quality control. Methods HPLC-CAD was used, chromatographic separation was performed on a Diamonsil C_(18) column(250 mm×4.6 mm, 5 μm). Acetonitrile(A)-0.05% ammonium acetate(acetic acid tone pH4.0)(B) was used as the mobile phase for gradient elution(0-10 min, 15% A; 10-25 min, 15%-30% A; 25-40 min, 30%-40% A; 40-50 min, 40%-70% A), the column temperature was maintained at 35 ℃, the nebulization temperature of detector was 35℃, the flow rate was 0.8 mL·min~(-1), and injection volume was 20 μL. The 6 components of Yuanhu Zhitong capsules were determined. Results The 6 components were linearity at 0.040-1.010 μg(r = 0.9991), 0.013-0.320 μg(r= 0.9994), 0.068-1.700 μg(r = 0.9994), 0.041-1.020 μg(r = 0.9997), 0.101-2.520 μg(r = 0.9991) and 0.039-0.980 μg(r = 0.9993), respectively. The average recoveries were 98.5%, 98.9%, 98.3%, 99.4%, 98.1% and 98.7%, and the RSDs were 0.90%, 1.4%, 0.70%, 1.1%, 0.70% and 0.90%. Conclusion The method is accurate, convenient and sensitive for the quality control of multicomponent of alkaloids and coumarins in Yuanhu Zhitong capsules.
引文
[1]中国药典2015年版.一部[S]. 2015:603-604.
[2]Yuan CS,Mehendale SR,Wang CZ,et al. Effects of Corydalis yanhusuo and Angelicae dahuricae on cold pressor-induced pain in Humans:A controlled trial[J]. J Clinic Pharmacol,2004,44(11):1323-1327.
[3]Chen YF,Tsai HY,Wu TS. Anti-inflammatory and analgesic activities from roots of Angelica pubescens[J]. Planta Med,1995,61(1):2-8.
[4]Zhang YC,Xu HY,Chen XM,et al. Study on the application of intestinal absorption in vitro coupled with bioactivity assessment in Yuanhu Zhitong preparation[J]. J Med Plants Res,2012,6(10):1941-1947.
[5]Leung WC,Zheng H,Huen MSY,et al. Anxiolytic-like action of orally administered dl-tetrahydropalmatine in elevated plus-maze[J]. Prog Neuro Psychoph,2003,27(5):775-779.
[6]张军荣,李建利. HPLC测定元胡止痛胶囊欧前胡素的研究[J].四川中医,2015,33(1):93-95.
[7]杨帆.改良高效液相色谱法测定元胡止痛滴丸和胶囊中延胡索乙素含量[J].中国药业,2014,23(13):24-25.
[8]何丹,杨林,张景. UPLC法测定元胡止痛胶囊中欧前胡素和异欧前胡素的含量[J].分析试验室,2013,32(10):87-90.
[9]杨芳,万丽,杨荣平,等.一测多评法测定元胡止痛胶囊中欧前胡素、异欧前胡素和延胡索乙素的含量[J].中国药房,2012,23(32):3046-3049.
[10]刘路,高旋,杨永健. HPLC-电雾式检测器的应用[J].中国医药工业杂志,2012,43(3):227-231.
[11]高维,方平飞,李焕德,等. HPLC-CAD法测定盐酸乙胺丁醇片中盐酸乙胺丁醇的含量[J].中南药学,2009,7(5):338-340.
[12]谭必琴,赵勇,刘雁鸣.高效液相色谱-电喷雾检测器法测定乳糖的含量及有关物质[J].中南药学,2017,15(9):1310-1313.
[13]张铁军,刘昌孝.中药五味药性理论辨识及其化学生物学实质表征路径[J].中草药,2015,46(1):1-6.
[14]刘昌孝,张铁军,何新,等.活血化瘀中药五味药性功效的化学及生物学基础研究的思考[J].中草药,2015,46(5):615-624.
[15]孙玉平,张铁军,曹煌,等.中药辛味药性表达及在临证配伍中的应用[J].中草药,2015,46(6):785-790.
[2]Yuan CS,Mehendale SR,Wang CZ,et al. Effects of Corydalis yanhusuo and Angelicae dahuricae on cold pressor-induced pain in Humans:A controlled trial[J]. J Clinic Pharmacol,2004,44(11):1323-1327.
[3]Chen YF,Tsai HY,Wu TS. Anti-inflammatory and analgesic activities from roots of Angelica pubescens[J]. Planta Med,1995,61(1):2-8.
[4]Zhang YC,Xu HY,Chen XM,et al. Study on the application of intestinal absorption in vitro coupled with bioactivity assessment in Yuanhu Zhitong preparation[J]. J Med Plants Res,2012,6(10):1941-1947.
[5]Leung WC,Zheng H,Huen MSY,et al. Anxiolytic-like action of orally administered dl-tetrahydropalmatine in elevated plus-maze[J]. Prog Neuro Psychoph,2003,27(5):775-779.
[6]张军荣,李建利. HPLC测定元胡止痛胶囊欧前胡素的研究[J].四川中医,2015,33(1):93-95.
[7]杨帆.改良高效液相色谱法测定元胡止痛滴丸和胶囊中延胡索乙素含量[J].中国药业,2014,23(13):24-25.
[8]何丹,杨林,张景. UPLC法测定元胡止痛胶囊中欧前胡素和异欧前胡素的含量[J].分析试验室,2013,32(10):87-90.
[9]杨芳,万丽,杨荣平,等.一测多评法测定元胡止痛胶囊中欧前胡素、异欧前胡素和延胡索乙素的含量[J].中国药房,2012,23(32):3046-3049.
[10]刘路,高旋,杨永健. HPLC-电雾式检测器的应用[J].中国医药工业杂志,2012,43(3):227-231.
[11]高维,方平飞,李焕德,等. HPLC-CAD法测定盐酸乙胺丁醇片中盐酸乙胺丁醇的含量[J].中南药学,2009,7(5):338-340.
[12]谭必琴,赵勇,刘雁鸣.高效液相色谱-电喷雾检测器法测定乳糖的含量及有关物质[J].中南药学,2017,15(9):1310-1313.
[13]张铁军,刘昌孝.中药五味药性理论辨识及其化学生物学实质表征路径[J].中草药,2015,46(1):1-6.
[14]刘昌孝,张铁军,何新,等.活血化瘀中药五味药性功效的化学及生物学基础研究的思考[J].中草药,2015,46(5):615-624.
[15]孙玉平,张铁军,曹煌,等.中药辛味药性表达及在临证配伍中的应用[J].中草药,2015,46(6):785-790.