HPLC波长切换法同时测定桂枝、白芍药对提取物中8个成分的含量

目的: 建立同时测定桂枝、白芍药对提取物中8个成分(没食子酸、氧化芍药苷、芍药内酯苷、芍药苷、1，2，3，4，6-五没食子酰葡萄糖、香豆素、肉桂酸、苯甲酰芍药苷) 含量的高效液相色谱法。方法: 采用Agilent Eclipse XDB-C₁₈色谱柱(250 mm×4.6 mm，5 μm)，以乙腈(A)-0.1%磷酸水溶液(B)为流动相，梯度洗脱，流速为1.0 mL·min^-1，检测波长为267 nm(0~13 min，检测没食子酸)、258 nm(13~20 min，检测氧化芍药苷)、230 nm(20~35 min，检测芍药内酯苷、芍药苷)、274 nm(35~47 min，检测1，2，3，4，6-五没食子酰葡萄糖)、280 nm(47~61 min，检测香豆素、肉桂酸)、230 nm(61~70 min，检测苯甲酰芍药苷)，柱温为30℃。结果: 桂枝、白芍药对提取物中8个成分没食子酸、氧化芍药苷、芍药内酯苷、芍药苷、1，2，3，4，6-五没食子酰葡萄糖、香豆素、肉桂酸、苯甲酰芍药苷进样量分别在0.0936~0.936 μg(r=0.9995)、0.005320~0.05320 μg(r=0.9991)、0.1365~1.365 μg(r=0.9996) 、0.1456~1.456 μg(r=0.9996)、 0.0939~0.939 μg(r=0.9997)、 0.02678~0.2678 μg(r=0.9992)、 0.1336~1.336 μg(r=0.9993)，0.01938~0.1938 μg(r=0.9992)与峰面积呈良好的线性关系；平均回收率(n=5)分别为99.8%、99.2%、99.0%、99.1%、98.3%、100.0%、98.1%、99.9% 。结论: 该方法准确可靠、重复性好，可用于桂枝、白芍药对提取物的质量控制。

Objective: To develop an HPLC method for determination of 8 indicative components (galic acid,oxypaeoniflorin,paeonilactone,paeoniflorin,1,2,3,4,6-pentagalloylglucose,cinnamic acid,coumarin,benzoylpaeoniflorin) in the extraction of drug-couple Persicae Ramulus and Paeoniae Radix Alba. Methods: The Agilent Eclipse XDB-C₁₈ column (250 mm×4.6 mm,5 μm) was adopted,the mobile phase was acetonitrile (A) - 0.1% phosphoric acid aqueous solution (B),with a gradient elution.The flow rate was 1.0 mL·min^-1,the detection wavelength was 267 nm (0-13 min) for galic acid,258 nm (13-20 min) for oxypaeoniflorin,230 nm (20-35 min) for paeonilactone and paeoniflorin,274 nm (35-47 min) for 1,2,3,4,6-pentagalloylglucose,280 nm (47-61 min) for cinnamic acid and coumarin,230 nm(61-70 min) for benzoylpaeoniflorin,and the column temperature was 30℃. Results: The injection volume of 8 indicative components in drug-couple Persicae Ramulus and Paeoniae Radix Alba had a good linearity in the ranges of 0.0936-0.936 μg (r=0.9995) for galic acid,0.005320-0.05320 μg (r=0.9991) for oxypaeoniflorin,0.1365-1.365 μg (r=0.9996) for paeonilactone,0.1456-1.456 μg (r=0.9996) for paeoniflorin,0.0939-0.939 μg (r=0.9997) for 1,2,3,4,6-pentagalloylglucose,0.02678-0.2678 μg (r=0.9992) for coumarin,0.1336-1.336 μg (r=0.9993) for cinnamic acid,0.01938-0.1938 μg (r=0.9992) for benzoylpaeoniflorin.The average recoveries (n=5) were 99.8%,99.2%,99.0%,99.1%,98.3%,100.0%,98.1%,99.9%,respectively.Conclusion: This method is accurate,reliable,repeatable,and can be used to control quality of the extraction of drug-couple Persicae Ramulus and Paeoniae Radix Alba.

1 XIE Ming(谢鸣).Prescriptions of Chinese Materia Medica(方剂学)[M].Beijing(北京)People's Medical Publishing House(人民卫生出版社),2002.43
2 YANG Song (杨松),JIA Ying (贾英),BI Kai-shun(毕开顺).RP-HPLC determination of 4 active components in Ramulus Cinnamomi(RP-HPLC法测定桂枝中4种活性成分的含量)[J].Chin J Pharm Anal(药物分析杂志),2004,24(2):143
3 ChP(中国药典)[S].2010.Vol Ⅰ(一部):96
4 LI Wei-ming(李伟铭),ZHAO Yue-ran(赵月然),YANG Yan-yun(杨艳云),et al.RP-HPLC with UV switch determination of 9 indicative components in white peony root pieces(HPLC波长切换法同时测定白芍饮片中9个成分的含量)[J].Chin J Pharm Anal(药物分析杂志),2011,31(12):2208