季正超,孙国祥
JI Zheng-chao,SUN Guo-xiang

• 1:沈阳药科大学药学院

摘要(Abstract)：

目的建立4波长复方丹参滴丸定量指纹图谱和同时测定8组分含量测定的分析方法,以综合评价复方丹参滴丸质量。方法采用色谱柱为Kromasil C_(18) BDS(250mm×4.6mm,5μm)柱,以5mmol·L~(-1)柠檬酸-10mmol·L~(-1)磷酸二氢钠(A)和体积分数1%醋酸乙腈(B)为流动相进行梯度洗脱,检测波长分别为270、280、290和326nm,流速为1mL·min~(-1),柱温为(35±0.1)℃,进样量为10μL,以反相高效液相色谱法建立4波长指纹图谱,同时测定8组分含量,用定量指纹图谱和8组分定量结果同时评价20批复方丹参滴丸质量。结果丹参素钠、原儿茶酸、原儿茶醛、咖啡酸、迷迭香酸、紫草酸、丹酚酸B和丹酚酸A分别在质量浓度为0.5~500、0.6~50、0.15~125、0.5~125、0.5~125、0.4~40、0.26~130和0.04~100mg·L~(-1)内呈良好线性关系(r>0.99),其检测限和定量限依次为0.15~1.5、0.02~0.6、0.02~0.15、0.03~0.15、0.03~0.15、0.4~40、0.03~0.08和0.02~0.12mg·L~(-1)。平均回收率在97.4%~103.4%内,RSD在0.92%~1.5%内(n=6)。20批样品宏定性相似度(S_m)均大于0.90,宏定量相似度(P_m)均在85%~115%内(α<0.15)。结论该方法为复方丹参滴丸的质量评价提供了新的参考。
Objective To evaluate the quality consistency of compound danshen dropping pills(CDDP) using 4 wavelength HPLC fingerprints combined with simultaneous determination of 8 components.Methods The Kromasil C_(18) BDS(250 mm×4.6 mm,5μm)was used for chromatographic system and the chromatographic separation was performed in gradient elution mode using 5 mmol·L~(-1) citric acid and 10 mmol·L~(-1) NaH_2PO_3(A)and a mixture of glacial acetic and acetonitrile in a ratio of 1∶100(V/V)(B)as mobile phrases.The column temperature was maintained at(35±0.1)℃.The flow rate and loading volume were set at 1.0mL·min~(-1) and10μL,respectively.Eight components in CDDP were determined simultaneously by standard curve method and chromatographic fingerprints were established at 270,280,290 and 326 nm for evaluating the quality of CDDP.Results The good linear ranges of 8 makers(salvianolic acid,protocatechuic acid,proticatechuic aldehyde,caffeic acid,rosmarinic acid,lithospermic acid,salvianic acid B,salvianolic acid A)were obtained in the range of0.5-500,0.6-50,0.15-125,0.5-125,0.5-125,0.4-40,0.26-130 and 0.04-100 mg·L~(-1) with the correlation coefficients higher than 0.99.The LOD and LOQ can be obtained using 3 times and10 times of the signal-to-noise(S/N)ratios,which were 0.15-1.5,0.02-0.6,0.02-0.15,0.03-0.15,0.03-0.15,0.4-40,0.03-0.08 and 0.02-0.12 mg·L~(-1),respectively.The average recoveries of 8 makers varied from97.4%to 103.4%and the relative standard deviations(RSD,n=6)were ranged from0.92%to 1.5%(n=6).The S_m and of 20 batches of CDDP were all more than 0.9 and below 0.15,and P_mwere all in the range of 85%-115%(α<0.15).Conclusions The method is simple and reasonable,which can be used as a novel reference to evaluate the quality of CDDP.

关键词(KeyWords)： 复方丹参滴丸;含量测定;高效液相指纹图谱;质量评价
compound Danshen dropping pills;content determination;HPLC fingerprint;quality assessment

Abstract:

Keywords:

基金项目(Foundation): 国家自然科学基金资助项目(90612002,81573586)

作者(Author): 季正超,孙国祥
JI Zheng-chao,SUN Guo-xiang

DOI: 10.14066/j.cnki.cn21-1349/r.2017.06.009

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