摘要
目的:建立纯化马钱子总生物碱HPLC指纹图谱,为其质量评价提供新方法。方法:采用HPLC测定纯化马钱子总生物碱中主要生物碱的含量,并考察其指纹图谱。含量测定的分析条件为Superstar C18色谱柱(4.6 mm×250 mm,5μm),流动相乙腈(A)-0.01 mol·L-11-庚烷磺酸钠与0.02 mol·L-1磷酸二氢钾等量混合(用10%磷酸调pH 2.8)(B)(24∶76),分析时间20 min,柱温30℃,检测波长264 nm;指纹图谱分析条件为Superstar C18色谱柱(4.6 mm×250 mm,5μm),流动相乙腈(A)-[水-三乙胺-乙酸(100∶0.2∶0.2)](B)进行梯度洗脱(0～21 min,10%～16%A;21～55 min,16%～40%A;55～65 min,10%A),分析时间65 min,柱温30℃,检测波长254 nm。结果:马钱子总生物碱的含量测定和指纹图谱分析各项参数均符合《中国药典》2010年版要求;10批纯化的马钱子总生物碱样品中含量分析显示,马钱子碱质量分数32.3%～37.5%,士的宁质量分数15.0%～18.4%,马钱子碱氮氧化物质量分数0.19%～0.23%;各批次样品的指纹图谱分析都显示10个共有峰,指纹图谱相似度均>97%。结论:含量测定与指纹图谱相结合的分析方法能很好地反映马钱子总生物碱的整体质量,纯化马钱子总生物碱的制备工艺稳定、重复性好,是一种有效的质量分析与评价方法。
Objective： To establish fingerprint of purified total alkaloids from processed Strychnos nux- vomica by HPLC-DAD, and provide a new method for quality control of S. nux-vomica. Method： The contents of brucine, strychnine and brucine N-oxide from purified total alkaloids of S. nux-vomica were determined by HPLC, and fingerprint was investigated. Analytical conditions of content determination were： Superstar C18 chromatographic column （4.6mm×250mm,5μm） , mobile phase of acetonitrile （A） -0.01 mol ~ L-I 1- heptane sulfonate and 0.02 mol-L-lpotassium dihydrogen phosphate mixed with equal amount （adjusted pH to 2.8 with 10% phosphonic acid） （24： 76） , analysis time 20 min, column tempreture 30℃ , detection wavelength at 264 nm; Analysis conditions of fingerprints were on Superstar Clschromatographic column （4.6mm×250mm,5μm）, acetonitrile （A） [ water-acetic acid-triethylamine （ 100： 0.2： 0.2） ] （B） as mobile phase with a method of gradient elution （0-21 min, 10%-16% A; 21-55 min, 16%40% A; 55-65 rain, 10% A） , parsing time 65 rain, column tempreture 30℃, UV detection wavelength at 254 nm. Result： Parameters of content determination and fingerprint analysis of total alkaloids from S. nux-vomica were in line with requirements of 2010 edition ＇ Chinese Pharmacopoeia＇ ; Content analysis of 10 batches of purified total alkaloids samples from S. nux- vomica showed that mass fraction of brucine, strychnine and brucine N-oxide were 32.3%-37.5%, 15.0%- 18.4% and 0.19% -0.23 % , respectively; Fingerprint analysis of each batch of samples showed 10 common peaks and fingerprint similarity were all above 97.0%. Conclusion： Combination of content determination and fingerprint could well reflect the overall quality of total alkaloids from S. nux-vomica, preparation process of depurated total alkaloids from processed S. nux-vomica was stable, reproducible, reliable, so it was an effective quality analysis and evaluation method.
出处
《中国实验方剂学杂志》
CAS
北大核心
2012年第22期76-80,共5页
Chinese Journal of Experimental Traditional Medical Formulae
基金
国家自然科学基金项目(30701111)
关键词
马钱子
纯化总生物碱
含量测定
指纹图谱
Strychnos nux-vomica
depurated total alkaloids
content determination
fingerprint
