The invention discloses a method for establishing UPLC fingerprint of compound Smilax granules and its fingerprint and application, which comprises the following steps: (1) sample preparation: (1) preparation of sample solution; (2) preparation of mixed reference solution; (2) UPLC fingerprint of compound Smilax granules extract: 2 mu L of sample solution and mixed reference solution are respectively injected into UPLC chromatographic analysis, and then UPLC chromatographic analysis is carried out. The chromatographic conditions were determined and the chromatograms were recorded for 38 minutes to obtain the fingerprints. The UPLC fingerprint of Compound Smilax Granules is established. Compared with HPLC, UPLC can ensure good separation of the extract of Compound Smilax Granules and greatly shorten the time of fingerprint analysis. The fingerprint composition of the compound Smilax granule of the invention is intact and has 18 common peaks, and the identification and attribution analysis are carried out. The separation effect of each characteristic peak is good, which can reflect the quality information of the product more comprehensively, and is conducive to the overall monitoring of product quality and the identification of the authenticity of the product.
【技术实现步骤摘要】
一种复方菝葜颗粒UPLC指纹图谱的建立方法及其指纹图谱与应用
本专利技术属于中药指纹图谱分析
,具体涉及一种复方菝葜颗粒UPLC指纹图谱的建立方法及其指纹图谱与应用。
技术介绍
指纹图谱是指某些复杂物质,比如中药,某种生物体或某种组织或细胞的DNA,蛋白质经适当处理后,采用一定的分析手段,得到的能够标示其化学特征的色谱图或光谱图。中药指纹图谱是一种综合的,可量化的鉴定手段,它是建立在中药化学成分系统研究的基础上,主要用于评价中药材以及中药制剂质量的真实性、优良性和稳定性。中药及其制剂均为多组分复杂体系,因此评价其质量应采用与之相适应的,能提供丰富鉴别信息的检测方法,建立中药指纹图谱将能较为全面地反映中药及其制剂中所含化学成分的种类与数量,进而对药品质量进行整体描述和评价。近年来,指纹图谱技术具有特征性强、专属性高、重现性好等优,已成功应用于评价植物药或中药质量的批次间稳定性。复方菝葜颗粒(compoundrhizomasmilacinusgranule,CRSG)是“湖南国华制药有限公司”具有告知只是产权的的独家抗肿瘤制剂,由菝葜、鱼腥草、猫爪草、款冬花、土鳖虫、枸杞子、大枣七味药和鲜鳢鱼组成,为临床癌症辅助治疗的常用药,具有清热解毒、软坚散结、滋阴益气等功效。该方组方精妙、疗效显著,方中菝葜、鱼腥草功善清热解毒、消痈排脓;猫爪草与土鳖虫配伍以软坚散结见长;枸杞子、大枣七味药和鳢鱼能补中益气、滋补生肌;款冬花则润肺下气,止咳化痰。全方合用,攻补兼施,标本同治,祛邪而不伤正,补虚而不滞腻,药性平和而又具有显著抗肿瘤作用。研究表明,CRSG具有抗炎、镇痛 ...
【技术保护点】
1.一种复方菝葜颗粒UPLC指纹图谱的建立方法,包括以下步骤:(1)样品的制备①供试品溶液配制:精密称取批复方菝葜颗粒1.0g,加甲醇定容至10mL,密闭,超声溶解,放冷,甲醇补足失重,摇匀,滤过,取滤液用0.22μm滤膜滤过,得到供试品溶液;②混合对照品溶液配制:取绿原酸、新绿原酸、隐绿原酸、异槲皮苷、金丝桃苷、落新妇苷、3,4‑二咖啡酰奎宁酸、3,5‑二咖啡酰奎宁酸,4,5‑二咖啡酰奎宁酸对照品适量,加适量甲醇制成含绿原酸90μg/mL、新绿原酸102.7μg/mL、隐绿原酸72.8μg/mL、金丝桃苷101.8μg/mL、落新妇苷133μg/mL、异槲皮苷104.8μg/mL、3,4‑二咖啡酰奎宁酸217.8μg/mL、3,5‑二咖啡酰奎宁酸93.2μg/mL,4,5‑二咖啡酰奎宁酸95.5μg/mL的混合对照溶液;(2)复方菝葜颗粒提取物UPLC指纹图谱将步骤1)中的供试品溶液和混合对照溶液,各取2μL,分别注入UPLC色谱分析,按照以下色谱条件进行测定,记录38min的色谱图,得到指纹图谱;色谱条件为:色谱柱为EC‑C18:3.0mm×50mm,2.7μm;检测波长280nm ...
【技术特征摘要】
1.一种复方菝葜颗粒UPLC指纹图谱的建立方法,包括以下步骤:(1)样品的制备①供试品溶液配制:精密称取批复方菝葜颗粒1.0g,加甲醇定容至10mL,密闭,超声溶解,放冷,甲醇补足失重,摇匀,滤过,取滤液用0.22μm滤膜滤过,得到供试品溶液;②混合对照品溶液配制:取绿原酸、新绿原酸、隐绿原酸、异槲皮苷、金丝桃苷、落新妇苷、3,4-二咖啡酰奎宁酸、3,5-二咖啡酰奎宁酸,4,5-二咖啡酰奎宁酸对照品适量,加适量甲醇制成含绿原酸90μg/mL、新绿原酸102.7μg/mL、隐绿原酸72.8μg/mL、金丝桃苷101.8μg/mL、落新妇苷133μg/mL、异槲皮苷104.8μg/mL、3,4-二咖啡酰奎宁酸217.8μg/mL、3,5-二咖啡酰奎宁酸93.2μg/mL,4,5-二咖啡酰奎宁酸95.5μg/mL的混合对照溶液;(2)复方菝葜颗粒提取物UPLC指纹图谱将步骤1)中的供试品溶液和混合对照溶液,各取2μL,分别注入UPLC色谱分析,按照以下色谱条件进行测定,记录38min的色谱图,得到指纹图谱;色谱条件为:色谱柱为EC-C18:3.0mm×50mm,2.7μm;检测波长280nm;柱温25℃;体积流量0.6ml/min;进样量2ul;流动相为A为甲醇,流动相B为0.3%甲酸水;梯度洗脱:0~2min,2%A,98%B;2~5min,2%~7%A,93%~98%B;5~12min,7%~11%A,89%~93%B;12~15min,11%~14%A,86%~89%B;15~17min,14%~16%A,84%~86%B;17~18min,16%~18%A,82%~84%B;18~20min,18%~20%A,80%~82%B;20~21min,20%~24%A,76%~80%B;21~24min,24%~26%A,74%~76%B;24~28min,26%~28%A,72%~74%B;28~29min,28%A,72%B;29~30min,28%~31%A,69%~72%B;30~35min,31%~48%A,52%~69%B;35~38min,48%A,52%B。2.根据权利要求1所述的指纹图谱的建立方法得到复方菝葜颗粒的UPLC指纹图谱。3.根据权利要求2所述的复方菝葜颗粒的UPLC指纹图谱,其特征在于,所述的指纹图谱共含有18个指纹峰,其相对保留时间分别为:1号峰:2.52;2号峰:2.746;3号峰:3....
【专利技术属性】
技术研发人员:朱立华,陈林,张水寒,胥新元,
申请(专利权)人:湖南国华制药有限公司,
类型:发明
国别省市:湖南,43
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