Objective

2

High performance liquid chromatography (HPLC) fingerprints of liposoluble and water-soluble fractions of Xiaojinwan were established and the similarity of fingerprints was evaluated

so as to explore the quality consistency of Xiaojinwan.

Method

2

Chromatographic separation was carried out on Welch Ultimate AQ-C

18

column (4.6 mm×250 mm

5 μm) with the mobile phase of 0.1% phosphoric acid solution (A)-acetonitrile (B) for gradient elution (liposoluble fraction of 0-5 min

40%B; 5-10 min

40%-50%B; 10-20 min

50%-60%B; 20-30 min

60%-65%B; 30-40 min

65%-70%B; 40-50 min

70%-80%B; 50-60 min

80%-90%B; 60-65 min

90%-95%B; 65-75 min

95%-100%B; 75-80 min

100%B; water-soluble fraction of 0-20 min

2%-5%B; 20-30 min

5%-10%B; 30-37 min

10%-20%B; 37-45 min

20%-30%B; 45-50 min

30%-40%B; 50-58 min

40%B)

the flow rate was 1 mL·min

-1

the column temperature was 30 ℃. The detection wavelengths of the liposoluble and water-soluble fractions were 202

250 nm

and their injection volumes were 10

20 μL

respectively. A total of 30 batches of Xiaojinwan from five manufacturers were detected by HPLC

the chromatographic peaks of each part were analyzed by principal component analysis (PCA) and identified.

Result

2

A total of 55 chromatographic peaks were detected in the fingerprints

and the similarity of fingerprint of 30 batches of Xiaojinwan was quite different. The relative standard deviations (RSDs) of fingerprint similarity of liposoluble and water-soluble fractions of Xiaojinwan were 21.5% and 32.8%

respectively. There were significant differences in the quality of samples from different manufacturers and the same manufacturer

and the chemical consistency evaluation results were dominated by liposoluble fraction

and the main reason for the chemical difference of this preparation was the composition of Liquidambaris Resina.

Conclusion

2

The quality consistency of Xiaojinwan is poor. The establishment of two-fraction fingerprint provides a new idea for the overall quality evaluation and control of Xiaojinwan

and can provide a reference for the quality consistency evaluation of traditional pills.