白芍药材和芍药籽饼粕中15种单萜苷含量测定

Simultaneous Determination of 15 Monoterpene Glycosides in Radix Paeoniae Alba and Seed Cake of Peony by HPLC

目的建立RP-HPLC同时测定白芍药材和芍药籽饼粕中15种单萜苷类化合物含量的方法。方法采用乙腈(A)和磷酸二氢钾缓冲盐(B)(pH 2.8)为流动相梯度洗脱,梯度为0 min(A,9%)→8 min(A,9%)→10 min(A,15%)→25 min(A,20%)→42 min(A,35%)→50 min(A,35%);检测波长:260 nm;柱温:30℃。结果吡啶芍药苷、牡丹皮苷F、氧化白芍苷、氧化芍药苷、10-羟基芍药苷、白芍苷、芍药苷、oxypaeonidanin、4-甲氧基-氧化芍药苷、没食子酰基芍药苷、4-甲氧基芍药苷、白芍苷R_1、paeonidanin、苯甲酰氧化芍药苷和苯甲酰芍药苷分别在5.1～81.6μg·mL^(-1)(r=0.999 3),12.95～207.2μg·mL^(-1)(r=0.999 9),6.2～99.2μg·mL^(-1)(r=0.998 8),12.2～195.2μg·mL^(-1)(r=0.999 1),8.0～128.0μg·mL^(-1)(r=0.999 7),5.5～88.0μg·mL^(-1)(r=1.000 0),6.0～96.0μg·mL^(-1)(r=0.999 5),6.0～96.0μg·mL^(-1)(r=0.999 6),5.6～89.6μg·mL^(-1)(r=0.993 2),4.7～75.2μg·mL^(-1)(r=0.999 8),5.4～86.4μg·mL^(-1)(r=1.000 0),5.0～80.0μg·mL^(-1)(r=1.000 0),5.7～91.2μg·mL^(-1)(r=1.000 0),5.4～86.4μg·mL^(-1)(r=1.000 0)和6.7～107.2μg·mL^(-1)(r=0.999 9)内有良好的线性关系;平均加样回收率为96.8%～105.6%,RSD在1.05%～3.41%。结论该方法准确,实用性好,可用于芍药药材和芍药籽饼粕中单萜苷类成分的定性与定量分析。

OBJECTIVE To establish an HPLC method for simultaneous determination of 15 monoterpene glycosides in Radix Paeoniae Alba and seed cake of peony.METHODS The separation was performed on an Agilent Zorbax SB C18-Aq column,using acetonitrile(A)and potassium dihydrogen phosphate solution(B)(p H 2.8)as the mobile phase by gradient elution.The elution program was as follows:0 min(A,9%)→8 min(A,9%)→10 min(A,15%)→25 min(A,20%)→42 min(A,35%)→50 min(A,35%).The flow rate was 1.0 mL·min-1.The detection wavelength was maintained at 260 nm.The column temperature was set at 30℃.RESULTS The linear range was 5.1-81.6μg·mL^-1 for pyrindylpaeoniflorin,12.95-207.2μg·mL^-1 for mudanpioside F,6.2-99.2μg·mL^-1 for oxyalbiflorin,12.2-195.2μg·mL^-1 for oxypaeoniflorin,8.0-128.0μg·mL^-1 for 10-hydroxypaeoniflorin,5.5-88.0μg·mL^-1 for albiflorin,6.0-96.0μg·mL^-1 for paeoniflorin,6.0-96.0μg·mL^-1 for oxypaeonidanin,5.6-89.6μg·mL^-1 for 4-O-methyl-oxypaeoniflorin,4.7-75.2μg·mL^-1 for galloylpaeoniflorin,5.4-86.4μg·mL^-1 for 4-O-methyl-paeoniflorin,5.0-80.0μg·mL^-1 foralbiflorin R1,5.7-91.2μg·mL^-1 for paeonidanin,5.4-86.4μg·mL^-1 for benzoyloxypaeoniflorin and 6.7-107.2μg·mL^-1 for benzoylpaeoniflorin.The average recoveries of the 15 monoterpene glycosides,were between 96.8%-105.6%and the RSD values were 1.05%-3.41%.CONCLUSION The method is simple,accurate and can be used for the quality control of peony.