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长春中医药大学药学院,长春 130117
Published:15 March 2023,
Received:09 September 2022,
Revised:06 February 2023,
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张静,孟灵旭,张洪涛等.一叶萩药材质量控制方法研究Δ[J].中国药房,2023,34(05):560-564.
ZHANG Jing,MENG Lingxu,ZHANG Hongtao,et al.Study on quality control method of Flueggea suffruticosa[J].ZHONGGUO YAOFANG,2023,34(05):560-564.
张静,孟灵旭,张洪涛等.一叶萩药材质量控制方法研究Δ[J].中国药房,2023,34(05):560-564. DOI: 10.6039/j.issn.1001-0408.2023.05.09.
ZHANG Jing,MENG Lingxu,ZHANG Hongtao,et al.Study on quality control method of Flueggea suffruticosa[J].ZHONGGUO YAOFANG,2023,34(05):560-564. DOI: 10.6039/j.issn.1001-0408.2023.05.09.
目的
2
建立一叶萩药材的质量控制方法。
方法
2
参照2020年版《中国药典》(四部)方法对一叶萩药材进行显微鉴别和薄层色谱(TLC)鉴别,并测定药材中的水分、总灰分及酸不溶性灰分、醇溶性浸出物;采用高效液相色谱(HPLC)法测定药材中一叶萩碱的含量。
结果
2
一叶萩药材的粉末呈灰绿色,气孔、花粉粒、草酸钙簇晶、导管等显微特征明显。TLC鉴别结果显示,16批药材样品的供试品色谱中,在与一叶萩碱、芦丁、槲皮素对照品及一叶萩对照药材色谱相应的位置上分别显相同颜色的斑点。16批药材样品的水分、总灰分、酸不溶性灰分、醇溶性浸出物的平均质量分数分别为9.26%、6.96%、1.17%、28.89%。一叶萩碱进样量在0.052 4~0.524 0 µg范围内与峰面积成良好的线性关系(
R
2
=0.999 8);精密度、重复性、稳定性(24 h)试验的RSD均小于3%(
n
为6或7);平均加样回收率为97.47%,RSD为1.63%(
n
=6)。16批药材样品中的一叶萩碱含量为1.003~6.872 mg/g。
结论
2
建立了一叶萩药材的质量控制方法,并初步拟定该药材中水分、总灰分及酸不溶性灰分分别不得过12.0%、9.0%、2.0%,醇溶性浸出物不得少于20%,一叶萩碱含量不得低于1.00 mg/g。
OBJECTIVE
2
To establish the quality control method of
Flueggea suffruticosa
.
METHODS
2
The microscopical identification and thin layer chromatography (TLC) of
F. suffruticosa
were carried out, and the mass fractions of moisture, total ash, acid-insoluble ash and alcohol-soluble extracts in
F. suffruticosa
were measured based on the 2020 version of
Chinese Pharmacopoeia
(part Ⅳ). The content of securinine in medicinal materials was determined by high performance liquid chromatography.
RESULTS
2
The powder of
F. suffruticosa
was gray-green, with obvious microscopic characteristics such as pores, pollen grains, calcium oxalate cluster crystals, ducts. The results of TLC identification showed that in the chromatograms of 16 batches of medicinal samples, the same color spots were found on the corresponding positions of the chromatograms of securinine, rutin, quercetin and
F. suffruticosa
control. The average mass fractions of moisture, total ash, acid-insoluble ash and alcohol-soluble extracts in 16 batches of medicinal materials were 9.26%, 6.96%, 1.17% and 28.89%, respectively. The injection volume of securinine in the range of 0.052 4-0.524 0 µg had a good linear relationship with the peak area (
R
2
=0.999 8). RSDs of precision, repeatability and stability (24 h) test were all less than 3% (
n
=6 or 7). The average recovery of sample was 97.47%, RSD was 1.63% (
n
=6). The content of securinine in 16 batches of medicinal materials was 1.003-6.872 mg/g.
CONCLUSIONS
2
The quality control method of
F. suffruticosa
is established, and the mass fractions of moisture, total ash and acid-insoluble ash should not exceed 12.0%, 9.0% and 2.0%, respectively; the alcohol-soluble extract should not be less than 20%, and the content of securinine should not be less than 1.00 mg/g.
一叶萩质量控制显微鉴别薄层色谱法高效液相色谱法一叶萩碱
quality controlmicroscopic identificationthin layer chromatographyhigh performance liquid chromatographysecurinine
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