ABSTRACT
AIM To establish an HPLC method for the simultaneous content determination of six constituents in Tibetan medicine Qishiwei Zhenzhu Pills (Croci Stigma,Dalbergiae odoriferae Lignum,Glycyrrhizae Radix et Rhizoma,etc.).METHODS The analysis of 50％ methanol extract of this drug was carried out on a 30 ℃ thermostatic Inertsil(C)ODS-3 column (250 mm ×4.6 mm,5 μm),with the mobile phase comprising of 0.2％ phosphoric acid-acetonitrile flowing at 0.8 mL/min in a gradient elution manner,and the detection wavelength was set at 254 nm.RESULTS Gallic acid,corilagin,agarotetrol,ellagic acid,crocin Ⅰ and crocin Ⅱ showed good linear relationships within the ranges of 1.41-42.24,0.61-18.24,0.30-9.12,0.47-14.04,0.62-18.48 and 0.32-9.45 μg/mL (R2 ≥0.999 4),whose average recoveries (RSDs) were 93.41％ (1.75％),96.84％ (1.75％),97.45％ (0.58％),93.22％ (0.56％),97.01％ (1.39％) and 97.22％ (1.11％),respectively.The contents of various constituents in different batches of samples from two manufactures showed some differences,especially for those of corilagin and agarotetrol.CONCLUSION We should pay attention to the unstable quality of Qishiwei Zhenzhu Pills.
ABSTRACT
AIM To establish an HPLC method for the simultaneous content determination of six constituents in Tibetan medicine Qishiwei Zhenzhu Pills (Croci Stigma,Dalbergiae odoriferae Lignum,Glycyrrhizae Radix et Rhizoma,etc.).METHODS The analysis of 50％ methanol extract of this drug was carried out on a 30 ℃ thermostatic Inertsil(C)ODS-3 column (250 mm ×4.6 mm,5 μm),with the mobile phase comprising of 0.2％ phosphoric acid-acetonitrile flowing at 0.8 mL/min in a gradient elution manner,and the detection wavelength was set at 254 nm.RESULTS Gallic acid,corilagin,agarotetrol,ellagic acid,crocin Ⅰ and crocin Ⅱ showed good linear relationships within the ranges of 1.41-42.24,0.61-18.24,0.30-9.12,0.47-14.04,0.62-18.48 and 0.32-9.45 μg/mL (R2 ≥0.999 4),whose average recoveries (RSDs) were 93.41％ (1.75％),96.84％ (1.75％),97.45％ (0.58％),93.22％ (0.56％),97.01％ (1.39％) and 97.22％ (1.11％),respectively.The contents of various constituents in different batches of samples from two manufactures showed some differences,especially for those of corilagin and agarotetrol.CONCLUSION We should pay attention to the unstable quality of Qishiwei Zhenzhu Pills.
ABSTRACT
This study was aimed to establish a quantitative method for the determination of agarotetrol in agarwood to control its quality. The HPLC analysis was performed on a Diamonsil C18 column (4.6 mm í 250 mm, 5 μm), eluted with a mobile phase of water with 0.1% formic acid and acetonitrile in gradient mode with the flow rate of 0.7 mL·min-1. The detection wavelength was set at 252 nm. The column temperature was 30oC. The results showed that the separation of agarotetrol and adjacent peaks were more than 1.5, which achieved a baseline separation. A good lin-earity (r = 0.999 8) was observed in the range of 2.0-125.0 μg·mL-1, with the average recovery of 102.75%. The a-garotetrol cannot be less than 0.15% based on the data of Agarwood samples. It was concluded that the method was accurate and reliable to determine the content of agarotetrol, which can be used for the quality control of agarwood.