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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 establish a method for the quantitative fingerprinting of 4-wavelength compound Danshen dropping pills and the simultaneous determination of 8 components in order to evaluate the quality of compound Danshen dripping pills. Methods The column was Kromasil C 18 BDS (250 mm × 4.6 mm, 5 μm) and the column was eluted with 5 mmol·L -1 citric acid -10 mmol·L -1 sodium dihydrogen phosphate (A) and volume The mobile phase was eluted with 1% acetonitrile (B) gradient. The detection wavelength was 270, 280, 290 and 326 nm, the flow rate was 1 mL · min -1 and the column temperature was 35 ± 0.1 ℃ The sample volume was 10 μL. The 4-wavelength fingerprinting was established by reversed-phase high performance liquid chromatography. The 8-component fingerprint was also determined. The quantitative fingerprint and 8-component quantitative results were used to evaluate the quality of 20 batches of compound Danshen dropping pills. Results Sodium danshensu, protocatechuic acid, protocatechuic aldehyde, caffeic acid, rosmarinic acid, lithospermate, salvianolic acid B and salvianolic acid A were respectively tested in the mass concentration of 0.5 ~ 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), and the limits of detection and quantification 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. The average recovery was within 97.4% to 103.4% with RSD within 0.92% to 1.5% (n = 6). The qualitative similarity (S_m) of all 20 batches of samples was greater than 0.90, and the macro quantitative similarity (P_m) was within 85% ~ 115% (α <0.15). Conclusion This method provides a new reference for the quality evaluation of compound Danshen dripping pills.