HPLC法同时测定复方元胡止痛片中6种成分
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摘要
目的建立HPLC法同时测定复方元胡止痛片(延胡索、香附、川楝子、徐长卿)中6种成分的含有量。方法该药物70%乙醇提取液的分析采用依利特C18色谱柱(250 mm×4.6 mm,5μm);以[甲醇-乙腈(1∶1)]-0.1%冰醋酸为流动相,梯度洗脱;体积流量1.2 m L/min;检测波长280 nm(原阿片碱、延胡索乙素、去氢紫堇碱、紫堇碱、四氢小檗碱)和242 nm(α-香附酮)。结果原阿片碱、延胡索乙素、去氢紫堇碱、紫堇碱、四氢小檗碱、α-香附酮分别在2.15~41.00μg/m L(r=0.999 9)、2.74~54.80μg/m L(r=0.999 8)、3.36~67.20μg/m L(r=0.999 6)、2.67~53.40μg/m L(r=0.999 5)、1.99~39.80μg/m L(r=0.999 7)、5.13~102.60μg/m L(r=0.999 8)范围内线性关系良好,平均加样回收率(RSD)分别为97.98%(1.13%)、99.12%(1.58%)、98.33%(0.83%)、99.05%(1.72%)、97.83%(1.42%)、98.64%(0.70%)。结论该方法准确可靠,专属性强,可用于复方元胡止痛片的质量控制。
AIM To establish an HPLC method for the simultaneous content determination of six constituents in Compound Yuanhu Zhitong Tablets( an analgesic containing Corydalis Rhizoma,Cyperi Rhizoma,Toosendan Fructus and Cynanchi paniculati Radix et Rhizoma). METHODS The analysis of 70% ethanol extract of this drug was performed on a Hypersil C18column( 250 mm × 4. 6 mm,5 μm),with the mobile phase comprising of methanol-acetonitrile( 1 ∶ 1)-0. 1% glacial acetic acid flowing at 1. 2 m L / min in a gradient elution manner,and the detection wavelengths were set at 280 nm for protopine,tetrahydropalmatine,dehydrocorydaline,corydaline and canadine, and 242 nm for α-cyperone. RESULTS Protopine,tetrahydropalmatine,dehydrocorydaline,corydaline,canadine and α-cyperone showed good linear relationships within the ranges of 2. 15- 41. 00 μg / m L( r = 0. 999 9),2. 74- 54. 80 μg /m L( r = 0. 999 8),3. 36- 67. 20 μg /m L( r = 0. 999 6),2. 67- 53. 40 μg /m L( r = 0. 999 5),1. 99- 39. 80 μg /m L( r = 0. 999 7) and 5. 13- 102. 60 μg /m L( r = 0. 999 8),whose average recoveries( RSDs) were 97. 98%( 1. 13%),99. 12%( 1. 58%),98. 33%( 0. 83%),99. 05%( 1. 72%),97. 83%( 1. 42%) and 98. 64%( 0. 70%),respectively. CONCLUSION With good specificity,this accurate and reliable method can be used for the quality control of Compound Yuanhu Zhitong Tablets.
AIM To establish an HPLC method for the simultaneous content determination of six constituents in Compound Yuanhu Zhitong Tablets( an analgesic containing Corydalis Rhizoma,Cyperi Rhizoma,Toosendan Fructus and Cynanchi paniculati Radix et Rhizoma). METHODS The analysis of 70% ethanol extract of this drug was performed on a Hypersil C18column( 250 mm × 4. 6 mm,5 μm),with the mobile phase comprising of methanol-acetonitrile( 1 ∶ 1)-0. 1% glacial acetic acid flowing at 1. 2 m L / min in a gradient elution manner,and the detection wavelengths were set at 280 nm for protopine,tetrahydropalmatine,dehydrocorydaline,corydaline and canadine, and 242 nm for α-cyperone. RESULTS Protopine,tetrahydropalmatine,dehydrocorydaline,corydaline,canadine and α-cyperone showed good linear relationships within the ranges of 2. 15- 41. 00 μg / m L( r = 0. 999 9),2. 74- 54. 80 μg /m L( r = 0. 999 8),3. 36- 67. 20 μg /m L( r = 0. 999 6),2. 67- 53. 40 μg /m L( r = 0. 999 5),1. 99- 39. 80 μg /m L( r = 0. 999 7) and 5. 13- 102. 60 μg /m L( r = 0. 999 8),whose average recoveries( RSDs) were 97. 98%( 1. 13%),99. 12%( 1. 58%),98. 33%( 0. 83%),99. 05%( 1. 72%),97. 83%( 1. 42%) and 98. 64%( 0. 70%),respectively. CONCLUSION With good specificity,this accurate and reliable method can be used for the quality control of Compound Yuanhu Zhitong Tablets.
引文
[1]中华人民共和国卫生部.卫生部颁药品标准(中药成方制剂):第7册[S].北京:人民卫生出版社,1993:123.
[2]国家药典委员会.中华人民共和国药典:2015年版一部[S].北京:中国医药科技出版社,2015:139-140,258.
[3]周卿,尚京川.HPLC-DAD法同时测定延胡索中4种生物碱的含量[J].重庆医科大学学报,2014,39(7):1017-1019.
[4]徐皓.HPLC法测定不同产地元胡药材中5种生物碱含量[J].药物分析杂志,2015,35(8):1403-1407.
[5]陈艳红,吴秋云,蔡佳仲.17批不同产地香附中有效成分的含量测定[J].临床医学工程,2010,17(11):41-42.
[6]王雪婷,宋德成,翟静,等.不同产地香附中α-香附酮含量测定[J].创新技术,2013(1):28-29.
[7]陈东东,毛坤军,李祥,等.HPLC法比较延胡索炮制前后7个生物碱成分的含量[J].药物分析杂志,2015,35(9):1591-1595.
[8]毕福钧,林彤.RP-HPLC法同时测定醋延胡索配方颗粒中7种生物碱[J].中草药,2016,47(4):606-609.
[9]冯自立,张涛,张晓娟,等.高效液相法测定陕西产延胡索中延胡索乙素,原阿片碱的含量[J].安徽农业科学,2009,37(21):9832-9833,9840.
[10]卢君蓉,傅超美,周莉江,等.香附醋制前后香附烯酮,圆柚酮和α-香附酮的含量比较[J].中国实验方剂学杂志,2014,20(20):24-27.
[11]季宁平,卢君蓉,盛菲亚,等.不同醋制方法对香附中指标成分含量的影响[J].中国实验方剂学杂志,2015,21(7):5-7.
[2]国家药典委员会.中华人民共和国药典:2015年版一部[S].北京:中国医药科技出版社,2015:139-140,258.
[3]周卿,尚京川.HPLC-DAD法同时测定延胡索中4种生物碱的含量[J].重庆医科大学学报,2014,39(7):1017-1019.
[4]徐皓.HPLC法测定不同产地元胡药材中5种生物碱含量[J].药物分析杂志,2015,35(8):1403-1407.
[5]陈艳红,吴秋云,蔡佳仲.17批不同产地香附中有效成分的含量测定[J].临床医学工程,2010,17(11):41-42.
[6]王雪婷,宋德成,翟静,等.不同产地香附中α-香附酮含量测定[J].创新技术,2013(1):28-29.
[7]陈东东,毛坤军,李祥,等.HPLC法比较延胡索炮制前后7个生物碱成分的含量[J].药物分析杂志,2015,35(9):1591-1595.
[8]毕福钧,林彤.RP-HPLC法同时测定醋延胡索配方颗粒中7种生物碱[J].中草药,2016,47(4):606-609.
[9]冯自立,张涛,张晓娟,等.高效液相法测定陕西产延胡索中延胡索乙素,原阿片碱的含量[J].安徽农业科学,2009,37(21):9832-9833,9840.
[10]卢君蓉,傅超美,周莉江,等.香附醋制前后香附烯酮,圆柚酮和α-香附酮的含量比较[J].中国实验方剂学杂志,2014,20(20):24-27.
[11]季宁平,卢君蓉,盛菲亚,等.不同醋制方法对香附中指标成分含量的影响[J].中国实验方剂学杂志,2015,21(7):5-7.