冯了性风湿跌打药酒的HPLC指纹图谱建立及其中10种有效成分的含量测定
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篇名: 冯了性风湿跌打药酒的HPLC指纹图谱建立及其中10种有效成分的含量测定
TITLE: Establishment of HPLC Fingerprints of Fengliaoxing Fengshi Dieda Wine and Content Determination of 10 Effective Components
摘要: 目的:建立冯了性风湿跌打药酒的高效液相(HPLC)指纹图谱,并测定其中10种有效成分的含量。方法:采用HPLC法。色谱柱为InertsilODS-3C18,流动相为乙腈-0.1%磷酸水溶液(梯度洗脱),流速为1.0mL/min,柱温为25℃,检测波长为210nm(10~15min,盐酸麻黄碱、盐酸伪麻黄碱)、300nm(70~120min,桂皮醛)、345nm(15~70min,新绿原酸、东莨菪苷、绿原酸、隐绿原酸、东莨菪内酯、异绿原酸A、异绿原酸C),进样量为10μL。以东莨菪内酯峰为参照,绘制10批样品的HPLC指纹图谱,采用《中药色谱指纹图谱相似度评价系统(2012版)》进行相似度评价,确定共有峰。结果:10批样品共有18个共有峰,相似度均大于0.980,共指认出盐酸麻黄碱、盐酸伪麻黄碱、新绿原酸、东莨菪苷、绿原酸、隐绿原酸、东莨菪内酯、异绿原酸B、柚皮苷、异绿原酸A、异绿原酸C、桂皮醛等12个成分。盐酸麻黄碱、盐酸伪麻黄碱、新绿原酸、东莨菪苷、绿原酸、隐绿原酸、东莨菪内酯、异绿原酸A、异绿原酸C、桂皮醛等10个成分检测质量浓度的线性范围分别为2.475~247.5、2.600~260.0、3.820~382.0、3.900~390.0、3.060~306.0、4.760~476.0、4.540~454.0、4.900~490.0、4.540~454.0、7.590~759.0μg/mL(r均大于0.9990);定量限分别为0.3200、0.3500、0.0214、0.0243、0.0368、0.0257、0.1521、0.0429、0.0251、0.3503μg/mL,检测限分别为0.1600、0.1800、0.0079、0.0040、0.0012、0.0073、0.0760、0.0014、0.0081、0.2014μg/mL;精密度、重复性、稳定性试验的RSD均小于2%;加样回收率为95.03%~106.85%(RSD为0.67%~2.68%,n=6);上述10种成分的含量分别为0.0133~0.2141mg/mL。结论:所建指纹图谱稳定、准确、专属性强,可用于冯了性风湿跌打药酒的质量控制;含量测定方法简便快速、准确可靠,可用于同时测定其中10种有效成分的含量。
ABSTRACT: OBJECTIVE:To establish an HPLC fingerprint for Fengliaoxing fengshi dieda wine ,and to determine the contents of 10 effective constituents. METHODS :HPLC method was adopted. The determination was performed on Inertsil ODS- 3 C18 column with mobile phase consisted of acetonitrile - 0.1% phosphoric acid water (gradient elution )at the flow rate of 1.0 mL/min. The column temperature was 25 ℃ ,and detection wavelength was set at 210 nm(10-15 min,hydrochloride ephedrine , hydrochloride pseudoephedrine ),300 nm(70-120 min,cinnamaldehyde),345 nm(15-70 min,neochlorogenic acid ,scopolin, chlorogenic acid ,cryptochlorogenic acid ,scopoletin,isochlorogenic acid A ,isochlorogenic acid C ). The sample size was 10 μL. Using scopoletin peak as reference ,HPLC fingerprints of 10 batches of samples were drawn. The similarity evaluation was performed by using Similarity Evaluation System of TCM Chromatographic Fingerprint (2012 edition)to confirm common peak. RESULTS:There were 18 common peaks in HPLC chromatograms of 10 batches of samples ,and the similarity was above 0.980. Totally 12 components including hydrochloride ephedrine , hydrochloride pseudoephedrine , neochlorogenic acid , scopolin, chlorogenic acid ,cryptochlorogenic acid ,scopoletin,isochlorogenic acid B ,narigin,isochlorogenic acid A ,isochlorogenic acid C and cinnamaldehyde widentified. The linear range of hydrochloride ephedrine ,hydrochloride pseudoephedrine ,neochlorogenic acid, scopolin, chlorogenic acid , cryptochlorogenic acid , scopoletin, isochlorogenic acid A , isochlorogenic acid C and cinnamaldehyde were 2.475-247.5,2.600-260.0,3.820-382.0,3.900-390.0,3.060-306.0,4.760-476.0,4.540-454.0,4.900-490.0, 4.540-454.0,7.590-759.0 μg/mL(r>0.999 0). The limits of quantitation were 0.320 0,0.350 0,0.021 4,0.024 3,0.036 8,0.025 7, 0.152 1,0.042 9,0.025 1,0.350 3 μg/mL,respectively;the limits of detection were 0.160 0,0.180 0,0.007 9,0.004 0,0.001 2, 0.007 3,0.076 0,0.001 4,0.008 1,0.201 4 μg/mL,respectively. RSDs of precision ,stability and reproducibility tests were all lower than 2%. The recoveries were 95.03%-106.85%(RSD were 0.67%-2.68%,n=6).The contents were 0.013 3- 0.214 1 mg/mL. CONCLUSIONS:Established fingerprint is stable ,accurate and specific ,and can be used for quality control of Fengliaoxing fengshi dieda wine ;the content determination method is rapid ,accurate and reliable ,and can be used for simultaneous determination of 10 components.
期刊: 2020年第31卷第08期
作者: 胡静,杨媛媛,崔小敏,任慧,雷琨,陈志永
AUTHORS: HU Jing,YANG Yuanyuan ,CUI Xiaomin ,REN Hui,LEI Kun,CHEN Zhiyong
关键字: 冯了性风湿跌打药酒;高效液相色谱法;指纹图谱;含量测定
KEYWORDS: Fengliaoxing fengshi dieda wine ;HPLC;Fingerprints;Content determination
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