贵州医科大学学报

2015, v.40;No.173(02) 142-145+158

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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
Rapid Extraction of Strychnine from Bitongning Capsule and Quantitative Detection by HPLC

徐纬;
XU Wei;School of Public Health,Guiyang Medical College;

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

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基金项目(Foundation): 贵阳医学院科研基金(K2009-31)

作者(Author): 徐纬;
XU Wei;School of Public Health,Guiyang Medical College;

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