Establishment of HPLC Fingerprints of Fengliaoxing Fengshi Dieda Wine and Content Determination of 10 Effective Components / 中国药房

ABSTRACT

OBJECTIVE：To establish an HPLC fingerprint for Fengliaoxing fengshi dieda wine ，and to determine the contents of 10 effective constituents. METHODS ：HPLC method was adopted. The determination was performed on Inertsil ODS- 3 C18 column with mobile phase consisted of acetonitrile - 0.1％ phosphoric acid water （gradient elution ）at the flow rate of 1.0 mL/min. The column temperature was 25 ℃ ，and detection wavelength was set at 210 nm（10-15 min，hydrochloride ephedrine ， hydrochloride pseudoephedrine ），300 nm（70-120 min，cinnamaldehyde），345 nm（15-70 min，neochlorogenic acid ，scopolin， chlorogenic acid ，cryptochlorogenic acid ，scopoletin，isochlorogenic acid A ，isochlorogenic acid C ）. The sample size was 10 μL. Using scopoletin peak as reference ，HPLC fingerprints of 10 batches of samples were drawn. The similarity evaluation was performed by using Similarity Evaluation System of TCM Chromatographic Fingerprint （2012 edition）to confirm common peak. RESULTS：There were 18 common peaks in HPLC chromatograms of 10 batches of samples ，and the similarity was above 0.980. Totally 12 components including hydrochloride ephedrine ， hydrochloride pseudoephedrine ， neochlorogenic acid ， scopolin， chlorogenic acid ，cryptochlorogenic acid ，scopoletin，isochlorogenic acid B ，narigin，isochlorogenic acid A ，isochlorogenic acid C and cinnamaldehyde widentified. The linear range of hydrochloride ephedrine ，hydrochloride pseudoephedrine ，neochlorogenic acid， scopolin， chlorogenic acid ， cryptochlorogenic acid ， scopoletin， isochlorogenic acid A ， isochlorogenic acid C and cinnamaldehyde were 2.475-247.5，2.600-260.0，3.820-382.0，3.900-390.0，3.060-306.0，4.760-476.0，4.540-454.0，4.900-490.0， 4.540-454.0，7.590-759.0 μg/mL（r＞0.999 0）. The limits of quantitation were 0.320 0，0.350 0，0.021 4，0.024 3，0.036 8，0.025 7， 0.152 1，0.042 9，0.025 1，0.350 3 μg/mL，respectively；the limits of detection were 0.160 0，0.180 0，0.007 9，0.004 0，0.001 2， 0.007 3，0.076 0，0.001 4，0.008 1，0.201 4 μg/mL，respectively. RSDs of precision ，stability and reproducibility tests were all lower than 2％. The recoveries were 95.03％-106.85％（RSD were 0.67％-2.68％，n＝6）．The contents were 0.013 3- 0.214 1 mg/mL. CONCLUSIONS：Established fingerprint is stable ，accurate and specific ，and can be used for quality control of Fengliaoxing fengshi dieda wine ；the content determination method is rapid ，accurate and reliable ，and can be used for simultaneous determination of 10 components.