ABSTRACT
In this experiment,the gradation analysis method was used to evaluate the quality of different pieces of Gardeniae Fructus through the extraction rate difference and the difference analysis of the main components in the extract. In this experiment cold-dip and hot-dip methods were used to compare the yield of Gardeniae Fructus extract and the content of chemical constituents with water,25%,50%,75% and 95% ethanol fractions. By weighted calculation,the optimal extraction method of Gardeniae Fructus was determined,and this was verified by practical application. RESULTS:: showed that for the water-soluble extract,cold dip method was better than the hot dip method; and for alcohol-soluble extract,75% ethanol under cold dip method was best. The verification results showed that water-soluble extracts under cold dip methods could be used to significantly distinguish the raw Gardeniae Fructus( GF) and processed( stir-baked) GF( GFP) collected from the market. Meanwhile,this method could be also used to distinguish the same batch of GF,GFP and carbonized GF( GFC) with significant differences,respectively( P<0. 05). Ethanol-soluble extract can be used to clearly distinguish GFP and GFC pieces in the same batch( P<0. 05). The results of content determination showed that the variation coefficient of components in GF processed products was higher than that in extracts,and the content of hydroxygeniposide was the most significant component between GF and its processed products. It is suggested that the method of water-soluble extract of GF and the determination of the content of gardoside should be combined together to evaluate the quality of GF and its heat processed products.
Subject(s)
Drugs, Chinese Herbal , Fruit , Chemistry , Gardenia , Chemistry , Plant ExtractsABSTRACT
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
OBJECTIVE:To establish the quality standard for Gardenia jasminoides. METHODS:The moisture,total ash and extract were determined. HPLC was used for contents determination of geniposide,rutin,crocinⅠand crocinⅡ:the column was Waters Xbridge-C18 with mobile phase of acetonitrile-0.2% phosphoric acid(gradient elution,gardenia and rutin),methanol-water (45∶55,V/V,crocinⅠ,crocinⅡ)at a flow rate of 1.0 ml/min;detection wavelength was 256 nm for gardenia and rutin,440 nm for crocinⅠ,crocinⅡ;column temperature was 30℃;injection volume was 10μl for gardenia and rutin,5μl for crocinⅠ,cro-cinⅡ. RESULTS:The moisture total ash and ethanol-soluble extract of G. jasminoides were 5.8%-8.4%,3.7%-5.9% and 29.5%-37.9%,respectively. The linear range was 162.08-1 620.84 μg/ml for geniposide(r=0.999 9),2.07-20.72 μg/ml for rutin (r=0.999 9),8.04-80.41 μg/ml for crocinⅠ(r=0.999 9)and 1.05-10.53 μg/ml for crocinⅡ(r=0.999 9);RSDs of precision,sta-bility and reproducibility test were lower than 2%;recoveries were 99.33%-101.43%(RSD=1.09%,n=6),97.97%-101.83%(RSD=1.39%,n=6),97.97%-101.30%(RSD=1.36%,n=6) and 98.65%-103.04%(RSD=1.84%,n=6). CONCLUSIONS:The established standard can be used for the quality control of G. jasminoides commercially available.