不同产地麸炒白术指纹图谱及同时测定3种白术内酯成分含量的方法研究
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摘要
目的采用高效液相色谱法建立41批不同产地麸炒白术药材的指纹图谱,并在指纹图谱条件下,同时测定3种白术内酯成分的质量分数。方法采用Phenomenex kinetex~@ XB C_(18)色谱柱(4.6 mm×250 mm,5μm),乙腈-水梯度洗脱,流速为0.8 m L/min,柱温为35℃,进样量为10μL,检测波长为220、242、278 nm。结果建立了41批不同产地麸炒白术药材的HPLC-DAD指纹图谱,并确立了指纹图谱的23个共有峰,指认了其中的白术内酯Ⅰ、白术内酯Ⅱ、白术内酯Ⅲ。白术内酯Ⅰ在131.38～394.13 ng、白术内酯Ⅱ在122.65～367.95 ng、白术内酯Ⅲ在181.38～545.5 ng范围内线性关系良好,r均大于0.999 0,平均加样回收率分别为100.62%、100.67%、99.51%,RSD分别为1.45%、1.97%、1.54%。结论建立的方法简单准确可靠,为评价和控制不同产地的麸炒白术药材质量提供了一定的科学依据。
Objective To establish an HPLC fingerprint method of Atractylodis Macrocephalae Rhizoma stirfried with wheat bran of 41 batches from different regions and determine the three contents in Microctis Folium( Atractylenolide Ⅰ; Atractylenolide Ⅱ; Atractylenolide Ⅲ). Methods It was detected with a Phenomenex kinetex@ XB-C_(18) column( 4.6 mm× 250 mm,5 μm),and gradually diluted with acetonitrilewater at a flow rate of 0.8 m L/min,the column temperature was 35 ℃,the injection volume was 10 μL,and the detection wavelength was set at 220,242,278 nm. Results A fingerprint of Atractylodis Macrocephalae Rhizoma stir-fried with wheat bran from different origins was established, and 23 common peaks were determined; Atractylenolide Ⅰ; Atractylenolide Ⅱ; Atractylenolide Ⅲ were baseline separated with good linearity relationships between concentration and peak areas over the linear ranges within 131.38-394.13 ng,122.65-367.95 ng,181.38-545.5 ng( r>0.999 0),whose average recoveries were 100.62%,100.67%,99.51% with RSD of 1.45%,1.97%,1.54%,respectively. Conclusion The established method is simple,accurate and reliable, which provides a scientific basis for evaluating and controlling the quality of Atractylodis Macrocephalae Rhizoma stir-fried with wheat bran from different regions.
Objective To establish an HPLC fingerprint method of Atractylodis Macrocephalae Rhizoma stirfried with wheat bran of 41 batches from different regions and determine the three contents in Microctis Folium( Atractylenolide Ⅰ; Atractylenolide Ⅱ; Atractylenolide Ⅲ). Methods It was detected with a Phenomenex kinetex@ XB-C_(18) column( 4.6 mm× 250 mm,5 μm),and gradually diluted with acetonitrilewater at a flow rate of 0.8 m L/min,the column temperature was 35 ℃,the injection volume was 10 μL,and the detection wavelength was set at 220,242,278 nm. Results A fingerprint of Atractylodis Macrocephalae Rhizoma stir-fried with wheat bran from different origins was established, and 23 common peaks were determined; Atractylenolide Ⅰ; Atractylenolide Ⅱ; Atractylenolide Ⅲ were baseline separated with good linearity relationships between concentration and peak areas over the linear ranges within 131.38-394.13 ng,122.65-367.95 ng,181.38-545.5 ng( r>0.999 0),whose average recoveries were 100.62%,100.67%,99.51% with RSD of 1.45%,1.97%,1.54%,respectively. Conclusion The established method is simple,accurate and reliable, which provides a scientific basis for evaluating and controlling the quality of Atractylodis Macrocephalae Rhizoma stir-fried with wheat bran from different regions.
引文
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[2]李尧,李伟,王琳,等.麸炒白术研究述要[J].山东中医药大学学报,2018,42(2):182-185.
[3]周文慧.姚乃礼教授辨治脾虚证的诊疗思路及临床经验[D].北京:北京中医药大学,2018.
[4]翁萍,王文凯,张晓婷.白术不同炮制品对脾虚小鼠胃肠功能的影响[J].江西中医药,2015,46(5):30-32.
[5]李滢,杨秀伟.麸炒白术化学成分的研究[J].中国现代中药,2018,20(9):1074-1079.
[6]徐春良,林苗苗,魏惠珍,等.不同炮制方法对白术药材指标成分含量及浸出物影响研究[J].江西中医药大学学报,2018,30(5):70-72.
[7]伍清芳,王智磊,鄢玉芬,等.白术麸炒过程中单糖和二糖组成及含量变化规律研究[J].成都中医药大学学报,2017,40(4):7-11.
[8]梁乙川,郭换,刘素娟,等.基于颜色变化的麸炒白术最佳炮制火候的客观量化判别[J].中国实验方剂学杂志,2018,24(6):12-15.
[9]黄妍,姚建标,赖云枫,等.麸炒白术配方颗粒特征图谱及白术内酯Ⅲ含量测定研究[J].中国现代应用药学,2017,34(9):1243-1247.
[10]潘欢欢.白术麸炒过程中物质基础、健脾作用和燥性变化研究[D].成都:成都中医药大学,2017.
[11]谌瑞林,何浪,费俗青,等.白术不同炮制品白术内酯含量的比较研究[J].时珍国医国药,2016,27(12):2911-2914.