HPLC Fingerprint Analysis of Liposoluble and Water-soluble Fractions of Xiaojinwan

Bi FENG; Jiao SONG; Zhi-min CI; Bo CAO; Hong XU; Xiao-juan DU; Jun-zhi LIN; Ding-kun ZHANG; Li HAN; Run-chun XU

doi:10.13422/j.cnki.syfjx.20201052

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HPLC Fingerprint Analysis of Liposoluble and Water-soluble Fractions of Xiaojinwan

Pharmacy Fundamentals | 更新时间：2020-09-09

- HPLC Fingerprint Analysis of Liposoluble and Water-soluble Fractions of Xiaojinwan
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 26, Issue 18, Pages: 139-144(2020)
- 作者机构：
  
  1.成都中医药大学药学院，成都 611137
  2.成都永康制药有限公司，成都 610041
  3.成都中医药大学附属医院，成都 610075
- 作者简介：
- 基金信息：
- DOI：10.13422/j.cnki.syfjx.20201052
  CLC： R22;R94;R28;C37;O657.7
- Received：12 December 2019，
  
  Published Online：05 February 2020，
  
  Published：20 September 2020
- 稿件说明：
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冯碧,宋娇,慈志敏等.小金丸脂溶性和水溶性部位的HPLC指纹图谱分析[J].中国实验方剂学杂志,2020,26(18):139-144.

FENG Bi,SONG Jiao,CI Zhi-min,et al.HPLC Fingerprint Analysis of Liposoluble and Water-soluble Fractions of Xiaojinwan[J].Chinese Journal of Experimental Traditional Medical Formulae,2020,26(18):139-144.
冯碧,宋娇,慈志敏等.小金丸脂溶性和水溶性部位的HPLC指纹图谱分析[J].中国实验方剂学杂志,2020,26(18):139-144. DOI： 10.13422/j.cnki.syfjx.20201052.

FENG Bi,SONG Jiao,CI Zhi-min,et al.HPLC Fingerprint Analysis of Liposoluble and Water-soluble Fractions of Xiaojinwan[J].Chinese Journal of Experimental Traditional Medical Formulae,2020,26(18):139-144. DOI： 10.13422/j.cnki.syfjx.20201052.

摘要

目的

建立小金丸脂溶性部位、水溶性部位的高效液相色谱法（HPLC）指纹图谱并进行指纹图谱相似度评价，探讨小金丸的质量一致性。

方法

采用Welch Ultimate AQ-C

色谱柱（4.6 mm×250 mm，5 μm），流动相选择0.1%磷酸水溶液（A）-乙腈（B）梯度洗脱（脂溶性部分：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。水溶性部分：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），流速1 mL·min

-1

，柱温30 ℃，脂溶性部位和水溶性部位的检测波长分别设定为202，250 nm，进样量依次为10，20 μL。对5个厂家共30批市售小金丸进行HPLC检测，使用主成分分析（PCA）对各部位色谱峰进行分析，并对色谱峰进行指认。

结果

指纹图谱共检测出55个色谱峰，30批小金丸指纹图谱相似度差异较大。小金丸脂溶性部位、水溶性部位的指纹图谱相似度RSD分别为21.5%和32.8%，厂家间与厂家内样品质量差异较大，且脂溶性部位成分主导小金丸化学一致性评价结果，其中，来自枫香脂的成分是影响该制剂化学差异的主要原因。

结论

市售小金丸质量一致性较差。双部位指纹图谱的建立为小金丸整体质量评控提供了新思路，可为传统丸剂的质量一致性评价提供参考。

Abstract

Objective

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

Chromatographic separation was carried out on Welch Ultimate AQ-C

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

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

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.

关键词

Keywords

references

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江宁 . 小金丸治疗良性前列腺增生80例 [J]. 世界中医药， 2008 ， 3 ( 5 )： 277 .

李慧芳 . 小金丸治疗带状疱疹后遗神经痛临床分析 [J]. 数理医药学杂志， 2018 ， 31 ( 4 )： 544 - 546 .

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熊茜，王小平，张定堃，等 . 基于粒子设计原理的中药制丸粉末中间体均一性优化与评价：以小金丸为例 [J]. 药学学报， 2017 ， 52 ( 10 )： 1611 - 1620 .

任桂林 . 粒子设计改善小金丸混合均匀性研究 [D]. 成都：成都中医药大学， 2015 .

CHOI J H ， PARK J K ， KIM K M ， et al . In vitro and in vivo antithrombotic and cytotoxicity effects of ferulic acid [J]. J Biochem Mol Toxicol ， 2018 ， 32 ( 1 )： e22004 .

FUKUDA T ， KURODA T ， KONO M ， et al . Augmentation of ferulic acid-induced vasorelaxation with aging and its structure importance in thoracic aorta of spontaneously hypertensive rats [J]. Naunyn Schmiedebergs Arch Pharmacol ， 2015 ， 388 ( 10 )： 1113 - 1117 .

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