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1.山西医科大学 药学院,太原 030001
2.中国中医科学院 中药研究所,北京 100700
肖鹿昆,硕士,从事药物分析研究,E-mail:xlk18417@163.com
张爱平,博士,教授,从事纳米材料的生物学效应研究,E-mail:zhangap1@163.com;
刘艳,博士,副研究员,从事中药质量控制技术和经典名方开发研究,E-mail:yliu1980@icmm.ac.cn
收稿日期:2023-02-08,
网络出版日期:2023-03-21,
纸质出版日期:2023-06-20
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肖鹿昆,赵桉熠,邸继鹏等.厚朴药渣资源化综合利用的预处理方法考察[J].中国实验方剂学杂志,2023,29(12):149-156.
XIAO Lukun,ZHAO Anyi,DI Jipeng,et al.Investigation of Pretreatment Methods for Comprehensive Resource Utilization of Magnoliae Officinalis Cortex Dregs[J].Chinese Journal of Experimental Traditional Medical Formulae,2023,29(12):149-156.
肖鹿昆,赵桉熠,邸继鹏等.厚朴药渣资源化综合利用的预处理方法考察[J].中国实验方剂学杂志,2023,29(12):149-156. DOI: 10.13422/j.cnki.syfjx.20230749.
XIAO Lukun,ZHAO Anyi,DI Jipeng,et al.Investigation of Pretreatment Methods for Comprehensive Resource Utilization of Magnoliae Officinalis Cortex Dregs[J].Chinese Journal of Experimental Traditional Medical Formulae,2023,29(12):149-156. DOI: 10.13422/j.cnki.syfjx.20230749.
目的
2
探究促进厚朴药渣酶解及有效成分提取的预处理方法,为厚朴药渣中资源性成分的利用提供参考依据。
方法
2
采用液质联用技术(LC-MS)分析厚朴药渣中资源性成分的种类,检测条件为Agilent C
18
反相色谱柱(3.0 mm×100 mm,2.7 µm),流动相水(A)-乙腈(B)梯度洗脱(0~3 min,25%~48%B;3~6 min,48%~59%B;6~10 min,59%~80%B;10~20 min,80%~90%B;20~25 min,90%B),流速0.4 mL·min
-1
,电喷雾离子源(ESI),负离子扫描模式,扫描范围
m
/
z
50~1 200。参考2020年版《中华人民共和国药典》(一部)“厚朴”项下含量测定方法,运用高效液相色谱法(HPLC)定量分析其资源性成分。采用4种预处理剂对厚朴药渣的资源性成分进行分离,并通过场发射扫描电子显微镜(FESEM)、X射线粉末衍射(XRD)及傅里叶变换红外光谱(FT-IR)技术分析不同预处理剂的作用机制。
结果
2
定性和定量分析明确了厚朴药渣的主要资源性成分为厚朴酚、和厚朴酚及木质纤维素组分。在1% NaOH、反应温度80 ℃、反应时间60 min条件下,预处理后固体残渣酶解产生还原糖质量浓度32.18 g·L
-1
,较未预处理药渣提高了79.8%,若加入聚山梨酯-80(tween-80),酶解时间缩至原来的1/3(24 h),还原糖质量浓度提高了102.0%;预处理液中厚朴酚及和厚朴酚的总回收率69.23%。
结论
2
厚朴药渣中厚朴酚、和厚朴酚及木质纤维素组分具备开发价值,碱预处理联合tween-80可实现这3种资源性成分的回收利用,可为中药药渣资源性成分的综合利用提供新思路。
Objective
2
To explore the pretreatment methods to promote the enzymatic digestion and extraction of active ingredients from Magnoliae Officinalis Cortex dregs(MOCD), and to provide a reference basis for the utilization of resource components in MOCD.
Method
2
Liquid chromatography-mass spectrometry(LC-MS) was used for qualitative analysis of resource components in MOCD with an Agilent C
18
reversed-phase column(3.0 mm×100 mm, 2.7 µm) at the flow rate of 0.4 mL·min
-1
, the mobile phase was water(A)-acetonitrile(B) for gradient elution(0-3 min, 25%-48%B; 3-6 min, 48%-59%B; 6-10 min, 59%-80%B; 10-20 min, 80%-90%B; 20-25 min, 90%B), electrospray ionization(ESI) was employed with negative ion mode scanning and scanning range of
m
/
z
50-1 200. A high performance liquid chromatography(HPLC), which refered to the determination in the 2020 edition of
Chinese Pharmacopoeia
, was used for quantitative analysis of resource components in MOCD. Four kinds of pretreatment agents were used to separate the resource components from MOCD, and the mechanism of different pretreatment agents was investigated by field emission scanning electron microscopy(FESEM), X-ray powder diffraction(XRD) and Fourier transform infrared spectroscopy(FT-IR).
Result
2
Magnolol, honokiol and lignocellulose were identified as the main resource components of MOCD by qualitative and quantitative analysis. Under the conditions of 1% NaOH, reaction temperature at 80 ℃ and reaction time of 60 min, the concentration of reducing sugar produced by the enzymatic hydrolysis was 32.18 g·L
-1
, which was 79.8% higher than that of the untreated MOCD. After adding tween-80, the enzymatic hydrolysis time was reduced to 1/3 of the original time, the concentration of reducing sugar was increased by 102.0%. And the total recovery of magnolol and honokiol in the pretreatment solution was 69.23%.
Conclusion
2
Magnolol, honokiol and lignocellulosic components in MOCD are valuable for development and utilization, the combination of alkaline pretreatment and tween-80 can realize the recovery and utilization of these three resource components, which can provide a new idea for comprehensive utilization of resource components in MOCD.
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