摘要
建立了超高效液相色谱(UPLC)测定制马钱子及其复方制剂痹祺胶囊、伸筋丹胶囊和晕复静片中士的宁和马钱子碱含量的方法。采用ZORBAX RRHD Eclipse Plus C_(18)色谱柱;流动相A为甲醇,流动相B为含1. 2%乙酸和0. 15%三乙胺的水溶液;流动相A-流动相B(24∶76,V/V)等度洗脱,流速0. 16 mL/min;检测波长260 nm。士的宁和马钱子碱分别在0. 49~19. 6μg/mL和0. 51~20. 4μg/mL的范围内线性良好;加样回收率均大于80. 0%,RSD均不超过2. 0%。本法准确度高,重复性好,专属性强,适用于制马钱子及其制剂的含量测定。
A method for determination of strychnine and brucine in processed strychnine semen and its preparations by ultra-performanceliquid chromatography( UPLC) was established. ZORBAX RRHDEclipse Plus C_(18) columnwas used,mobile phase Awas methanol and mobile phase B was solution of 1. 2% acetic acid and 0. 15% triethylamine. An isocratic elutionwas carried out using mobile phase A-mobile phase B( 24 ∶ 76, V/V). The flow rate was 0. 16 mL/min,detection wavelength was 260 nm. There was a good linear relationship of strychnine in the range of 0. 49 ~ 19. 6 μg/mL( R=0. 9997) and strychnine in the range of 0. 51~20. 4 μg/mL( R=0. 9998). The recoveries were above 80. 0%. RSD values were not more than 2. 0%. The proposed method was accurate and reproducible,which can be used for the assay of processed strychnine semen and its compound preparation.
引文
[1] GUO R, WANG T, ZHOU G, et al. Botany, Phytochemistry,Pharmacology and Toxicity of Strychnosnux-vomica L.:A Review[J].The American Journal of Chinese Medicine,2018,46(1):1-23.
[2]史磊,李永吉,裴丽,等.马钱子的本草考证[J].现代中药研究与实践,2017,31(06):6-10.
[3]张莉,李莉,杜冠华.中药马钱子毒的历史认识与现代研究[J].中药药理与临床,2018,34(04):191-194.
[4]刘轶凡,赵进喜,梁晓东.马钱子减毒增效配伍方法初探[J].中国医院药学杂志,2018,38(24):2612-2614.
[5]王咏,陈军.马钱子总生物碱含量测定方法的建立与比较[J].西部中医药,2017,30(07):29-32.
[6]姜林,李茜,齐雪梅.复方马钱子胶囊质量标准研究[J].新疆中医药,2006(01):39-40.
[7]王继芬,王朝虹,赵敬真,等. HPLC、GC法分析士的宁、马钱子碱[J].中国人民公安大学学报(自然科学版),2004(02):10-11.
[8]段存贤,郭承军. HPLC法测定神农丸中士的宁与马钱子碱的含量[J].药物分析杂志,2018,38(02):331-335.
[9]王竞,吴敏,孙成均,等.胶束毛细管电泳在线推扫法测定中成药中的士的宁[J].华西药学杂志,2012,27(05):560-562.
[10]国家药典委员会.中华人民共和国药典(一部)[S].北京:中国医药科技出版社,2015:975.
[11]张铮. HPLC法测定晕复静片中士的宁和马钱子碱的含量[J].安徽医药,2003,7(3):214-216.