Study On Quality Control Of Xuefuzhuyu Pill And Determination Of Metal Elements

Xuefuzhuyu pill was reported originally in yilingaicuo,written by Wang Qingren.This paper is about the extraction process and quality assessment and the study of constant & metal elements,which is composed of Semen Persicae,Flos Carthami,Radix Angelicae Sinensis,Radix Rehmanniae,Rhizoma Chuanxiong,Radix Paeoniae Rubra,Radix Achyranthis Bidentatae,Radix Platycodi,Radix Bupleuri,Fructus Aurantii and Radix Glycyrrhizae.The optimal alcohol extraction process of Xuefuzhuyu pill was studied by orthogonal design with extractive yield and the contents of hydro-saffior yellow A,paeoniflorin,ferulic acid and hesperidin from Xuefuzhuyu pill as quality assessment indices.Three factors were studied in this experiment,including the methanol consumption,duration of extration and times of extration.The results showed that the optimal extraction condition was methanol consumpted 20 times the amount of material,refluxing for once and 1 hour per time.RP-HPLC methods were established to simultaneously determine hydro-saffior yellow A in Carthamus tinctorius L.,paeoniflorin in Radix Paeoniae Alba,ferulic acid in Radix Angelicae Sinensis and Radix Ligusticum wallichii Franch.,hesperidin in Poncirus trifoliata (L.)Rafi and Citrus aurantium L..The separatior of four marker compounds was achieved on a Kromasil C₁₈column(250 mmx4.6 mm,5μm)with gradient elution using solvents of acetonitrile and aqueous acetic acid.The detection wavelength was set at 265 nm and the flow rate was 1.0 mL·min^-1.Assay was linear over the range 23.85～119.3μg·mL^-1for hydro-safflor yellow A(r=0.9996),140～644μg·mL^-1for paeoniflorin(r=0.9992),10.25～47.15μg·mL^-1for ferulic acid(r=0.9993),130～598μg·mL^-1for hesperidin(r=1.0). Average recoveries of samples were 99.8%(RSD=1.4%),100.3%(RSD=0.3%),96.6% (RSD=2.0%)and100.4%(RSD=1.0%)for four constituents,respectively.Three herbs of Xuefuzhuyu pill were indentified by TLC with the dots clear and reproducible.The assay methods were accurate and with good reproducibility and provided a quantitative basis for the quality assessment for Xuefuzhuyu pill.FAAS methods were also established to simultaneously determine Ca,Mg,Zn,Cu,Fe,Mn,Ni,Cr.The samples were digested with HNO₃-HCLO₄(4:1,v/v)at 140℃under normal pressure.Assay was linear over the range 23.85～119.3μg·mL^-1for hydro-safflor yellow A(r=0.9996),1.0～8.0μg·mL^-1for Ca(r=0.9994),0.1～3.0μg·mL^-1for Mg(r=0.9995), 0.3～2.0μg·mL^-1for Zn(r=0.9995),0.1～0.5μg·mL^-1for Cu(r=0.9993),0.5～6.01μg·mL^-1for Fe(r=1.0),0.1～1.6μg·mL^-1for Mn(r=0.9996),0.1～0.5μg·mL^-1for Ni(r=0.9992),0.05～0.4μg·mL^-1for Cr(r=1.0).Average recoveries of samples were 100.2%(RSD =1.5%), 98.4%(RSD=2.7%),104.5%(RSD =4.4%),101.8%(RSD =2.3%),101.5%(RSD =3.0 %),103.9%(RSD=3.2%),104.7%(RSD=4.5%)and 102.3%(RSD=2.3%)for eight elements,respectively.The assay methods were accurate,rapid and simple,providing a quantitative basis for the quality assessment for Xuefuzhuyu pill in another way and providing a basis to study the relationship between elements and diseases.