基于UHPLC-ELSD指纹图谱及多成分含量测定比较不同产地羊胆汁质量及抗氧化活性

Comparison of the Quality of Sheep Bile from Different Regions Based on UHPLC-ELSD Fingerprint and Multi-component Content Determination Combined with Antioxidant Activity

关键词:  羊胆汁  指纹图谱  含量测定  抗氧化活性  熵权TOPSIS  灰色关联度  质量控制

Key words:  sheep bile  fingerprint  content determination  antioxidant activity  entropy weight TOPSIS  grey correlation analysis  quality control

摘要:

目的 建立UHPLC-ELSD指纹图谱与多成分含量测定方法，比较不同产地羊胆汁的差异，并进行抗氧化活性研究，为羊胆汁的深入开发利用提供依据。方法 采用UHPLC-ELSD建立21批不同产地羊胆汁指纹图谱并进行相似度分析；测定6个成分含量、DPPH及ABTS自由基清除能力、铁离子还原能力，并进行熵权TOPSIS及灰色关联度分析。结果 21批羊胆汁指纹图谱共确定11个共有峰，通过与对照品比对指认出牛磺胆酸(taurocholic acid，TCA)、甘氨胆酸(glycocholic acid，GCA)、牛磺鹅脱氧胆酸(taurochenodeoxycholic acid，TCDCA)、牛磺脱氧胆酸(tauroursodeoxycholic acid，TDCA)、甘氨脱氧胆酸(glycodeoxycholic acid，GDCA)、胆酸(cholic acid，CA) 6个成分，除4批样品外，指纹图谱相似度均>0.90，21批羊胆汁冻干粉中6个成分的总含量范围为55.34%~86.08%，含量最高的TCA含量范围为34.74%~60.86%，显示6个成分含量在不同产地样品中存在较大差异；不同产地羊胆汁均具有抗氧化活性，同样也存在一定差异。以6个成分含量为变量的熵权TOPSIS分析结果显示，得分排名位于前十的为S2、S18、S16、S9、S8、S21、S1、S10、S20、S15，表明其质量较好，且来自北方地区绵羊的羊胆汁质量略优；对6个成分含量与3个抗氧化指标的灰色关联度分析结果显示，6个成分与各抗氧化指标均具有关联性，且TCA、TDCA、TCDCA关联度最高，可能是羊胆汁发挥抗氧化作用的重要成分。结论 采用熵权TOPSIS及灰色关联度分析方法能有效分析不同产地羊胆汁的质量差异及抗氧化活性成分，为其质量评价提供科学依据。

Abstract:

OBJECTIVE To establish UHPLC-ELSD fingerprint and multi-component content determination methods, compare the differences in sheep bile from different regions, and conduct antioxidant activity research to provide a basis for the in-depth development and utilization of sheep bile. METHODS Used UHPLC-ELSD method to establish 21 batches of bile fingerprints of sheep from different origins and conduct similarity analysis. Measured the content of 6 components, DPPH and ABTS free radical scavenging ability, iron ion reduction ability, and conducted entropy weighted TOPSIS and grey correlation analysis. RESULTS A total of 11 common peaks were identified in the fingerprint spectra of 21 batches of sheep bile. Through comparison with the control sample, 6 components were identified, including taurocholic acid(TCA), glycocholic acid(GCA), taurochenodeoxycholic acid(TCDCA), tauroursodeoxycholic acid(TDCA), glycodeoxycholic acid(GDCA), and cholic acid(CA). Except for 4 batches of samples, the similarity of the fingerprint spectra was greater than 0.90. The total content range of 6 components in the freeze-dried powder of 21 batches of sheep bile was 55.34% to 86.08%. The highest content of taurocholic acid ranged from 34.74% to 60.86%, indicating significant differences in the content of the six components in samples from different regions. Sheep bile from different regions had antioxidant activity, and there were also certain differences. The results of entropy weighted TOPSIS analysis using six component contents as variables showed that the top ten scoring groups were S2, S18, S16, S9, S8, S21, S1, S10, S20, and S15, indicating good quality and slightly better bile quality from sheep in the northern region. The grey correlation analysis results between the content of 6 components and 3 antioxidant indicators showed that all 6 components were correlated with each antioxidant indicator, and TCA, TDCA, and TCDCA had the highest correlation, which might be important components for sheep bile to exert antioxidant effects. CONCLUSION The use of entropy weighted TOPSIS and grey correlation analysis methods can effectively analyze the quality differences and antioxidant active components of sheep bile from different regions, providing scientific basis for its quality evaluation.