Content Determination of 10 Kinds of Chemical Components in Ligusticum chuanxiong under Different Storage Conditions by HPLC / 中国药房

ABSTRACT

OBJECTIVE： To establish the method for the content determination of chlorogenic acid， ligustrazine， ferulic acid， senkyunolide I， senkyunolide H， coniferly ferulate， senkyunolide A， n-butylphtalide， Z-ligustilide and n-butylidenephthalide in Ligusticum chuanxiong under different storage conditions. METHODS： HPLC method was adopted. The determination was performed on Boston C18 column with mobile phase consisted of acetonitrile-0.5％ acetic acid solution （gradient elution） at the flow rate of 1.0 mL/min. The detection wavelength was set at 285 nm， and the column temperature was 30 ℃. The sample size was 5 μL. RESULTS： The linear range of chlorogenic acid， ligustrazine， ferulic acid， senkyunolide I， senkyunolide H， coniferly ferulate， senkyunolide A， n-butylphtalide， Z-ligustilide n-butylidenephthalide were 0.030 53-0.519 01 μg （r＝0.999 5）， 0.001 02-0.017 34 μg （r＝0.999 9）， 0.012 83-0.218 11 μg （r＝0.999 5）， 0.007 63- 0.129 71 μg （r＝0.999 7）， 0.001 76-0.029 92 μg （r＝0.999 5）， 0.054 74-0.930 58 μg （r＝0.999 9）， 0.215 80-3.668 60 μg （r＝0.999 9）， 0.018 02-0.306 34 μg （r＝0.999 7）， 0.232 50- 3.952 50 μg （r＝0.999 9）， 0.002 40-0.040 80 μg （r＝0.999 5）.The limits of quantitation were 2.073 7， 0.556 6， 0.753 8， 0.231 5， 0.306 9， 0.925 2， 2.295 3， 4.624 0， 3.215 3， 0.910 5 ng， respectively. The detection limits were 0.622 1， 0.167 0， 0.226 1， 0.069 4， 0.092 1， 0.277 6， 0.688 6， 1.387 2， 0.964 6， 0.273 1 ng， respectively. RSD of precision， stability and repeatability tests were all less than 5％ （n＝6）. The recovery rates were 95.90％-103.28％ （RSD＝2.99％， n＝6）， 88.24％-107.84％ （RSD＝4.89％， n＝6）， 95.06％-102.08％ （RSD＝3.97％， n＝6）， 93.67％-101.05％ （RSD＝1.02％， n＝6）， 94.81％-104.33％ （RSD＝2.34％，n＝6）， 94.41％-105.59％ （RSD＝4.32％， n＝6）， 92.76％-104.83％ （RSD＝1.95％， n＝6）， 87.22％-102.56％ （RSD＝2.89％， n＝6）， 94.04％-99.52％ （RSD＝0.92％， n＝6）， 88.51％-103.83％ （RSD＝4.89％， n＝6）， respectively. At 5 ℃ and 15 ℃， no obvious deterioration was observed in medicinal materials. At room temperature， some samples were moth-eaten and mildewed. The content ranges of 6 batches of samples were 0.047 7％-0.160 8％， 0.006 1％- 0.022 7％， 0.048 2％-0.172 2％， 0.023 3％-0.145 2％， 0.004 6％-0.030 7％， 0.085 2％-0.835 4％， 0.182 6％-2.112 7％， 0.009 9％- 0.098 3％， 0.614 9％-3.176 2％ and 0.005 7％-0.036 9％， showing decreasing trend； the decrease rate was in descending order 5 ℃＜15 ℃＜room temperature； at the same storage temperature， the decrease rate of polyethylene plastic bag was lower than that of polypropylene woven bag. CONCLUSIONS： This method is accurate and feasible， and can be used for simultaneous determination of 10 kinds of components in L. chuanxiong. It is suggested that L. chuanxiong medicinal materials should be sealed and packed in dry and cool places and should not be stored for a long time.