ABSTRACT
Objective To improve the quality of aiye processed products, an eucalyptol content in commercially available aiye two processed products of chao aiye and aiye tan was investigated.Methods A capillary gas chromatography was used.The sample was prepared with n-hexane by reflux condensation.Chromatographic conditions: The separation was carried on an Ailgent DB-1 capillary column(30 mm ×0.320 mm ×0.25 μm). Inlet temperature was 200℃ and FID temperature was 250℃.The programmed column temperature was set as follows:maintained at 100℃ for 6 min and raised to 160℃ at the rate of 20℃/min followed by holding for 3min.The splitting-ratio was 5.0:1.The carried gas was nitrogen, flow rate was 1.0 mL/min.Injection volume was 1μL.Results In the given chromatographic conditions, the eucalyptol chromatographic separation had good, and the separation degree was greater than 1.5 between eucalyptol and other impurity peak.The linear range of eucalyptol was 11.4-114.0 mg/mL(r=0.999 5). Methods repeatability and recovery were good.The minimum limit of quantification was 0.5μg/mL.The results of determination of eucalyptol show that the eucalyptol content in the commercially available 11 batch of chao aiye was between 5.6-78.2 μg /g, and 12 batch of aiye tan had no eucalyptol. Conclusion The processing technology of current commercially available aiye processed products of chao aiye and aiye tan need to be improved, and the quality standard need to be improved.
ABSTRACT
[Objective]To observe the indexes of quality control of nature and quantity of Yanluotong Infusion.[Method]Make authentication to the 2 main components of Ligusticum wallichii and rhizoma sparganii on their nature with Silica gel G thin-layer chromatography;make content measurement to puerarin with RP-HPLC,take Kromasil 100-5 C18(4.6mm?250mm,5?m)as chromatogram column,methanol-water(30:70)as flow phase;the measured wavelength is 250nm.[Result]The puerarin sampling in the range 0.06~0.65?g is in good linear relationship with the summit area,the relative coefficient r=0.9999,the intraday and days nicety RSD are respectively 0.85% and 0.48%(n=5);the average sample reclaim rates of high,middle and low concentrations(n=3)are respectively 101.2%,101.1% and 101.4%,RSD is 1.1%,0.94% and 0.41% separately.[Conclusion]Silica gel G thin-layer chromatography and RP-HPLC are correct and reliable for nature and quantity control,with good repeatability,and can be taken as quality control standard of the preparation.
ABSTRACT
OBJECTIVE: To establish headspace capillary gas chromatography for the content determination of 3 kinds of residual organic solvent (furanidine,methanol and ethanol) in betamethasone sodium phosphate raw material.METHODS: The sample was dissolved in water and n-propanol was used as internal standard.The residual solvent in betamethasone sodium phosphate was separated on HP-INNOWAX (PEG) capillary column with column temperature set at 60 ℃.The injector temperature and FID detector temperature were controlled at 180 ℃ and 250 ℃,respectively.The carried gas was nitrogen at flow rate of 1.0 mL?min-1.The splitting-ratio was 10 ∶ 1.The containers of head-space injector were in equilibrium at 80 ℃ for 30 min.Injection time was 1 min.RESULTS: With this chromatographic condition,those solvents could be separated completely.The linear range were 0.014 4～0.071 8 mg?mL-1 for furanidine,0.060～0.300 mg?mL-1 for methanol and 0.099 3～0.497 mg?mL-1 for ethanol.The average recovery were 103.7% (RSD=0.53%,n=6),95.8% (RSD=0.30%,n=6) and 95.0% (RSD=0.48%,n=6) respectively.The minimum quantitation limit were 0.057 3 ?g?mL-1,0.486 ?g?mL-1,0.145 ?g?mL-1,respectively.3 kinds of residual organic solvents were all in line with the standard stated in Chinese Pharmacopeia.CONCLUSION: The established method is simple,sensitive and accurate for the content determination of residual solvents in betamethasone sodium phosphate raw material.