徐纬
XU Wei

• 1:贵阳医学院公共卫生学院

摘要(Abstract)：

目的:建立痹痛宁胶囊中士的宁的快速提取与高效液相色谱法定量检测的方法。方法:样品用甲醇-水-浓盐酸(50∶50∶1)溶液超声提取30 min,提取液稀释处理后,应用高效液相色谱法,采用Eclipse XDB C18柱(150 mm×4.6 mm×5μm),柱温25℃,0.01 mol/L庚烷磺酸钠与0.02 mol/L磷酸二氢钾等量混合,用10%磷酸调节p H 2.8后,与乙晴按79∶21比例混合作为流动相,流速1.0 m L/min,在260 nm波长下进行测定。结果:士的宁峰与相邻峰完全分离,进样量在0.02~1.00μg与峰面积呈良好的线性关系(r=1.000 0),方法检测限为0.002μg,平均回收率为(101.8±2.9)%(n=9),相对标准偏差RSD小于3%。结论:高效液相色谱法定量检测痹痛宁胶囊中士的宁含量具有快速、准确、灵敏度高、操作简便等优点。
Objective: To establish the method to rapidly extract strychnine from Bitongning capsule and using high performance liquid chromatography( HPLC) for quantitative detection. Methods: The extraction sample was ultrasonicly extracted for 30 min by methanol-H2O-HCL( 50∶ 50∶ 1),the diluted extracting solution was determined by HPLC,Eclipse XDB C18column( 150 mm × 4. 6 mm × 5 μm)was used,the column temperature was 25 ℃,with mobile phase a mixed solution of equal amount of acetonitrile- 0. 01 mol / L sodium heptanesulfonate and 0. 02 mol / L potassium dihydrogen phosphate( p H was adjusted to 2. 8 by 10% phosphoric acid)( 21∶ 79),the flow rate was 1. 0 m L/min and detected under the wave length of 260 nm. Results: The strychnine peak and the adjacent peak were separated fully,the injection volume was in the range of 0. 02 ~ 1. 00 μg,shared good linear relationship with the peak area,r = 1. 000 0,the method detection limit was 0. 002 μg,the average recovery rate was( 101. 8 ± 2. 9) %( n = 9),the RSD was less than 3%. Conclusions: This method was rapid,accurate,sensitive and simple.

关键词(KeyWords)： 士的宁;痹痛宁胶囊;色谱法,高压液相
strychnine;bitongning capsule;chromatography,high pressare lipuid

Abstract:

Keywords:

基金项目(Foundation): 贵阳医学院科研基金(K2009-31)

作者(Author): 徐纬
XU Wei

DOI: 10.19367/j.cnki.1000-2707.2015.02.012

参考文献(References)：

• [1]李阳,薛丰,王媛,等.高效毛细管电泳法同时测定减肥类功能食品中7种违禁成分[J].分析化学,2011(11):1716-1720.
• [2]陆小洁,段玺,宋逍.紫外分光光度法测定平消胶囊中士的宁含量[J].陕西中医学院学报,2009(1):72-73.
• [3]林昱,李新田,邱财荣,等.薄层扫描法测定接骨丹胶囊中士的宁[J].中国实验方剂学杂志,2010(7):53-54.
• [4]YBZ11142005.国家食品药品监督管理局标准(试行)[S].
• [5]吕霞,郭青,钟文英.GC-MS法测定疏风活络丸中伪麻黄碱、麻黄碱、士的宁和马钱子碱的含量[J].中国药科大学学报,2008(6):519-522.
• [6]国家药典委员会.中华人民共和国药典(一部)[M].北京:中国医药科技出版社,2010:48.
• [7]王蕾.RP-HPLC测定痹痛宁胶囊中士的宁和马钱子碱的含量[J].药学与临床研究,2012(4):377-378.
• [8]孙笑嫚,高鹏.高效液相色谱法测定痹痛宁胶囊中士的宁的含量[J].时珍国医国药,2006(3):359-360.
• [9]王东平.高效液相色谱法测定风湿痹康胶囊中士的宁含量[J].长春中医药大学学报,2011(5):847-848.
• [10]刘建,韩凤梅,陈勇.高效液相色谱法测定痹祺胶囊中马钱子碱、士的宁和丹酚酸B[J].分析化学,2009(4):609-612.
• [11]GB/T 24800.7-2009.化妆品中马钱子碱和士的宁的测定-高效液相色谱法[S].
• [12]魏秀德,杨波,范里,等.马钱子生物碱提取工艺的研究[J].吉林农业大学学报,2011(2):195-198.
• [13]汤淮波,张令君,李湘玲,等.不同溶剂提取马钱子中士的宁与马钱子碱的实验研究[J].中医药导报,2009(11):52-53.

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