ABSTRACT
OBJECTIVE To establish an HPLC fingerprint of Xiao’er resuqing oral liquid， and to determine the contents of twelve index components. METHODS HPLC method was adopted. The determination was performed on Venusil MP C18 column with mobile phase consisting of acetonitrile-0.1% phosphate aqueous solution （gradient elution） at a flow rate of 1.0 mL/min. The detection wavelength was set at 210 nm， the column temperature was 30 ℃， the injection volume was 10 μL. HPLC fingerprint of Xiao’er resuqing oral liquid was established by using the Similarity Evaluation System of Chromatographic Fingerprint of TCM （2012 edition） to evaluate the similarity. The contents of 12 components were determined， including （R， S）-goitrin， 3，5-O-dicaffeoyl quinic acid， puerarin， forsythin， forsythoside A， chlorogenic acid， baicalin， saikosaponins d， wogonoside， baicalein， emodin and chrysophanol. RESULTS The similarity of HPLC fingerprints of 13 batches of Xiao’er resuqing oral liquid was greater than 0.97， and 14 common peaks were confirmed. The contents of the above 12 index components in 13 batches of Xiao’er resuqing oral liquid were as follows： 0.078-0.172， 1.564-2.736， 1.338-2.578， 0.426-0.872， 1.477-2.628， 1.396-2.447， 4.052-9.146， 0.367- 0.692， 1.974-4.674， 1.274-2.969， 0.085-0.167 and 0.155-0.307 mg/mL. CONCLUSIONS The established HPLC fingerprint and content determination methods have high accuracy and high specificity， which can be used for the quality evaluation of Xiao’er resuqing oral liquid.
ABSTRACT
OBJECTIVE： To establish a method for simultaneous determination of 6 components in Chaihuang tablets， such as baicalin， wogonoside， baicalein， wogonin， saikosaponin a and saikosaponin d in Chaihuang tablets. METHODS： HPLC-DAD method was used to detect 3 batches of Chaihuang tablets from same manufacturers. The determination was performed on Agilent Eclipse XDB-C18 column with mobile phase consisted of acetonitrile-triethylamine phosphate aqueous solution （pH adjusted to 7.0， gradient elution） at flow rate of 1.0 mL/min. The detection wavelengths were set at 210 nm （saikosaponin a， saikosaponin d） and 277 nm （baicalin， wogonoside， baicalein， wogonin）. The column temperature was 30 ℃， and sample size was 5 μL. RESULTS： The linear ranges of baicalin， wogonoside， baicalein， wogonin， saikosaponin a and saikosaponin d were 0.379 5-7.590 4 μg， 0.082 96-1.659 2 μg， 0.039 39-0.787 8 μg， 0.040 72-0.814 4 μg， 0.040 45-0.809 0 μg， 0.038 63-0.772 6 μg （all r≥0.999 3）， respectively. The limits of detection were 0.008， 0.007， 0.005， 0.005， 0.020 and 0.018 μg/mL. The limits of quantitation were 0.025， 0.022， 0.015， 0.015， 0.060， 0.054 μg/mL. RSDs of precision， reproducibility and stability tests （48 h） were all lower than 1.5％ （n＝6）. Average recoveries were 98.46％， 97.06％， 100.90％， 96.13％， 96.91％， 96.57％ （RSD＜2.0％， n＝6）. CONCLUSIONS： Established method is simple， accurate and reproducible for 6 components in Chaihuang tablets， and can be used for quality control of the tablet.
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OBJECTIVE:To establish a method for simultaneous determination of pulchinenoside B4,caffeic acid,baicalin, palmatine hydrochloride and berberine hydrochloride in Baipuhuang tablets. METHODS:HPLC method was adopted. The determi-nation of Agela Technologies Venusil XBP C18(L)with mobile phase consisted of acetonitrile-0.05 mol/L monopotassium phosphate (gradient elution)at the flow rate of 0.8 mL/min. The detection wavelengths were set at 203 nm(pulchinenoside B4)and 323 nm (caffeic acid,baicalin,palmatine hydrochloride,berberine hydrochloride). The column temperature was set at 30 ℃,and the sam-ple size was 10 μL. RESULTS:The linear ranges were 0.08141-8.141μg for pulchinenoside B4(r=0.9998),0.01871-1.871 μg for caffeic acid (r=0.9994),0.03733-3.733 μg for baicalin (r=0.9992),0.02885-2.885 μg for palmatine hydrochloride (r=0.9996) and 0.02758-2.758 μg for berberine hydrochloride (r=0.9997). The limits of quantitation were 0.009,0.006,0.008, 0.011,0.013 ng,respectively. The limits of detection were 0.030,0.020,0.025,0.034,0.036 ng,respectively. RSDs of preci-sion,stability and reproducibility tests were all lower than 2.0%. The average recoveries were 97.39%-102.34%(RSD=1.81%,n=6),96.77%-98.92%(RSD=0.85%,n=6),97.38%-103.72%(RSD=2.46%,n=6),96.73%-102.01%(RSD=2.22%,n=6)and 96.47%-101.07%(RSD=1.61%,n=6),respectively. CONCLUSIONS:The method is simple,accurate and reproducibility,and can be used for simultaneous determination of pulchinenoside B4,caffeic acid,baicalin,palmatine hydrochloride and berberine hy-drochloride in Baipuhuang tablet.
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Objective:To establish the HPLC fingerprint of ethanol parts of compound Sanhuang tincture ( an anti-infective drug) using high performance liquid chromatography, and analyze the classification of the chemical components. Methods: A Phenomenex Luna C18 (2) (250 mm × 4. 6 mm, 5 μm) column was used. The mobile phase was acetonitrile-0. 05 mol·L-1 aqueous potassium di-hydrogen phosphate solution (22 :78) and the flow rate was 1. 0 ml·min-1 . The DAD detector was used and the detection wavelength was 237 nm. The column temperature was 30 ℃ and the injection volume was 10 μl. Results:The fingerprints of compound Sanhuang tincture were obtained with promising separation degree and the number of theoretical plates. A total of six fingerprint characteristic peaks were identified, and the reproducibility, stability and precision of the method were good. Meanwhile, combined with the informa-tion of retention time of compound medicine, single drug and reference substance, the source of characteristic peak of the effective part of compound Sanhuang tincture was determined. Conclusion:The fingerprints of compound Sanhuang tincture have strong characteris-tics and good reproducibility, which have important reference value for the quality evaluation of ethanol parts of compound Sanhuang tincture.