白芍药材和芍药籽饼粕中15种单萜苷含量测定
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摘要
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 R_1,5.7-91.2μg·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.
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 R_1,5.7-91.2μg·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.
引文
[1]Nanjing University of Chinese Medicine.The Dictionary of Chinese Herbal Medicine(中国中药大辞典)[M].Shanghai:Shanghai Scientific&Technical Publishers,2012:946-949.
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[3]MA L,LI Z X.Immunomodulatory effects and chinical application of total glucosides of peony[J].J Exp Tradit Med Form(中国实验方剂学杂志),2010,16(17):244-246.
[4]ZHANG L F,LIU Y M,PAN H M,et al.Pharmacokinetic study of total glucosides of paeony in immunological liver injured rats[J].Chin Pharmacol Bull(中国药理学通报),2011,27(10):1462-1466.
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[6]LIU Y L,LV J H.Hypolipidemic and antioxidative effect and hepatic protective effect of totalglucosides of peony on non-alcoholic fatty liver[J].J Hainan Med Univ(海南医学院学报),2012,18(2):158-161.
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[9]SHI X H,MA G Y,JIN L,et al.Fruit setting characteristics of ten peony oil varieties in Hangzhou[J].J Zhejiang Agr Sci(浙江农业科学),2017,58(3):459-462.
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[11]MA G Y,SHI X H,ZOU Q C,et al.Characters determination of herbaceous oil physicochemicalproperty and comparative analysis of Peony seed oil[J].J Chin Cereal Oil Assoc(中国粮油学报),2017,32(3):130-134.
[12]LUO J.Optimization of ultrasonic-assisted extraction of oil from seed of Paeonia lactiflora Pall and chemical composition of the seed cake[D].Luoyang:Master's Degree Thesis of Henan University of Science and Technology,2015.
[13]LIU P,XUY F,GAOX D,et al.Optimization of ultrasonic-assisted extraction of oil from the seed kernels and isolation of monoterpene glycosides from the oil residue of Paeonia lactiflora Pall[J].Ind Crop Prod,2017,107:260-270.
[14]WU S H,WUD G,CHENY W.Chemical constituents and bioactivities of plants from the genus Paeonia[J].Chem Biodivers,2010,7(7):90-104.
[15]HE C N,PENG Y,ZHANG Y C,et al.Phytochemical and biological studies of Paeoniaceae[J].Chem Biodivers,2010,7(7):805-838.
[16]LIU P,LI X F,ZHANG H,et al.RP-HPLC Simultaneous determination of six monoterpene glycosides in seed cake and seed shell of Peony for oil[J].J Chin Cereal Oil Assoc(中国粮油学报),2016,31(10):142-145.
[17]LIU P,ZHANG Y,GAO J Y,et al.HPLC-DAD analysis of 15monoterpene glycosides in oil peony seed cakes sourced from different cultivation areas in China[J].Ind Crop Prod,2018,118:259-270.
[18]LI W M,ZHAO Y Y,YANG Y Y,et al.RP-HPLC with UVswitch determination of 9 components in white peony root pieces[J].Chin J Pharm Anal(药物分析杂志),2011,31(12):2208-2212.
[19]GE Z W,HE Q,LIN Y J,et al.RP-HPLC Determination of albiflorin,paeoniflorin,and benzoylpaeoniflorin in Paeonia lactiflora and its prepared slices[J].Chin Tradit Herb Drugs(中草药),2008,39(3):378-380.
[20]HE X J,ZHANG Z Q,WANG J N,et al.HPLC with UVswitch determination of 8 indicative components in combination extracts of Persicae Ramulus and Paeoniae Radix Alba[J].Chin J Pharm Anal(药物分析杂志),2013,33(11):1899-1903.
[21]WANG Q,LIU R X,BI K S,et al.HPLC Determination of albiflorin,paeoniflorin,and benzoylpaeoniflorinin total glucoside of Paeony capsule[J].Chin Tradit Herb Drugs(中草药),2005,36(11):1630-1632.
[22]LIU P,ZHANG Y,XU Y F,et al.Three new monoterpene glycosides from oil peony seed cake[J].Ind Crop Prod,2018,111:371-378.
[2]LIU H Z,LIU A R,LI X L,et al.The chemical composition and pharmacodynamics research recent development about peeled root of Herbaceous Peony[J].J Anhui Technical Teachers College(安徽技术师范学院学报),2001,15(4):54-57.
[3]MA L,LI Z X.Immunomodulatory effects and chinical application of total glucosides of peony[J].J Exp Tradit Med Form(中国实验方剂学杂志),2010,16(17):244-246.
[4]ZHANG L F,LIU Y M,PAN H M,et al.Pharmacokinetic study of total glucosides of paeony in immunological liver injured rats[J].Chin Pharmacol Bull(中国药理学通报),2011,27(10):1462-1466.
[5]ZHANG J J,HUANG Y F,WANG L L,et al.Comparative study on effects of blood enriching on mouse model of blood deficiency syndrome induced by compound method of bleeding,starved feeding and exhausting of Paeoniae Radix Alba and Paeoniae Radix Rubra,paeoniflorin and albiflorin[J].China J Chin Med Mater(中国中药杂志),2013,38(19):3358-3362.
[6]LIU Y L,LV J H.Hypolipidemic and antioxidative effect and hepatic protective effect of totalglucosides of peony on non-alcoholic fatty liver[J].J Hainan Med Univ(海南医学院学报),2012,18(2):158-161.
[7]TONG H Y,SHUI Y X.42 Cases of juvenile rheumatoid arthritis treated with capsule of total glycosides of Paeonia[J].Zhejiang J Tradit Chin Med(浙江中医杂志),2009,44(7):543-543.
[8]BAI F L,ZHAO B.Clinical study of total glycosides of Paeonia in the treatment of rheumatoid arthritis[J].Helongjiang Med J(黑龙江医学),2014,38(7):835-835.
[9]SHI X H,MA G Y,JIN L,et al.Fruit setting characteristics of ten peony oil varieties in Hangzhou[J].J Zhejiang Agr Sci(浙江农业科学),2017,58(3):459-462.
[10]LIU P,LI X F,LIU Y Q,et al.Optimization of ultrasound-assisted aqueous extraction of oil from Paeonia lactiflora Pall.seed[J].China Oils Fats(中国油脂),2016,41(5):1-5.
[11]MA G Y,SHI X H,ZOU Q C,et al.Characters determination of herbaceous oil physicochemicalproperty and comparative analysis of Peony seed oil[J].J Chin Cereal Oil Assoc(中国粮油学报),2017,32(3):130-134.
[12]LUO J.Optimization of ultrasonic-assisted extraction of oil from seed of Paeonia lactiflora Pall and chemical composition of the seed cake[D].Luoyang:Master's Degree Thesis of Henan University of Science and Technology,2015.
[13]LIU P,XUY F,GAOX D,et al.Optimization of ultrasonic-assisted extraction of oil from the seed kernels and isolation of monoterpene glycosides from the oil residue of Paeonia lactiflora Pall[J].Ind Crop Prod,2017,107:260-270.
[14]WU S H,WUD G,CHENY W.Chemical constituents and bioactivities of plants from the genus Paeonia[J].Chem Biodivers,2010,7(7):90-104.
[15]HE C N,PENG Y,ZHANG Y C,et al.Phytochemical and biological studies of Paeoniaceae[J].Chem Biodivers,2010,7(7):805-838.
[16]LIU P,LI X F,ZHANG H,et al.RP-HPLC Simultaneous determination of six monoterpene glycosides in seed cake and seed shell of Peony for oil[J].J Chin Cereal Oil Assoc(中国粮油学报),2016,31(10):142-145.
[17]LIU P,ZHANG Y,GAO J Y,et al.HPLC-DAD analysis of 15monoterpene glycosides in oil peony seed cakes sourced from different cultivation areas in China[J].Ind Crop Prod,2018,118:259-270.
[18]LI W M,ZHAO Y Y,YANG Y Y,et al.RP-HPLC with UVswitch determination of 9 components in white peony root pieces[J].Chin J Pharm Anal(药物分析杂志),2011,31(12):2208-2212.
[19]GE Z W,HE Q,LIN Y J,et al.RP-HPLC Determination of albiflorin,paeoniflorin,and benzoylpaeoniflorin in Paeonia lactiflora and its prepared slices[J].Chin Tradit Herb Drugs(中草药),2008,39(3):378-380.
[20]HE X J,ZHANG Z Q,WANG J N,et al.HPLC with UVswitch determination of 8 indicative components in combination extracts of Persicae Ramulus and Paeoniae Radix Alba[J].Chin J Pharm Anal(药物分析杂志),2013,33(11):1899-1903.
[21]WANG Q,LIU R X,BI K S,et al.HPLC Determination of albiflorin,paeoniflorin,and benzoylpaeoniflorinin total glucoside of Paeony capsule[J].Chin Tradit Herb Drugs(中草药),2005,36(11):1630-1632.
[22]LIU P,ZHANG Y,XU Y F,et al.Three new monoterpene glycosides from oil peony seed cake[J].Ind Crop Prod,2018,111:371-378.