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米炒北沙参的质量标准研究
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| 篇名： | 米炒北沙参的质量标准研究 |
| TITLE： | Study on quality standard for rice-fired Glehnia littoralis |
| 摘要： | 目的 建立米炒北沙参的质量标准。方法取米炒北沙参饮片样品，进行外观性状观察、粉末显微鉴别、薄层色谱（TLC）鉴别，按2020年版《中国药典》（四部）通则方法检测其中水分、总灰分、酸不溶性灰分、水溶性浸出物及酸溶性浸出物的含量，采用高效液相色谱（HPLC）法测定其中补骨脂素、花椒毒素、佛手柑内酯、欧前胡素、异欧前胡素的含量。结果米炒北沙参饮片为类圆形小段，略粗糙，表面呈黄色（去皮）或深黄棕色（有皮），气特异，味微甘。其粉末呈黄白色，显微镜下可见分泌物和分泌细胞、导管、糊化淀粉粒、射线细胞、薄壁细胞等。TLC图斑点清晰，供试品色谱中，在与异欧前胡素对照品色谱相应的位置上，显相同的蓝色荧光斑点。9批米炒北沙参饮片的水分含量为5.82％～6.27％，总灰分含量为3.19％～3.59％，酸不溶性灰分含量为0.21％～0.27％，水溶性浸出物含量为24.91％～30.30％，醇溶性浸出物含量为20.66％～25.83％。补骨脂素、花椒毒素、佛手柑内酯、欧前胡素、异欧前胡素检测质量浓度的线性范围分别为0.240～2.400、0.320～3.200、0.224～2.240、0.292～2.920、0.208～2.080μg/mL（r均大于0.9990）；定量限分别为0.0320、0.0300、03250、0.0320、0.0450µg，检测限分别为0.1008、0.0896、0.0715、0.0900、0.1320µg；精密度、稳定性（24h）、重复性试验的RSD均小于3％；平均加样回收率分别为100.56％（RSD＝1.36％，n＝6）、100.73％（RSD＝2.25％，n＝6）、100.36％（RSD＝0.98％，n＝6）、98.24％（RSD＝0.40％，n＝6）、99.40％（RSD＝0.35％，n＝6）。上述5个成分的含量分别为5.85～13.31、8.63～33.38、6.23～15.25、6.12～12.98、5.52～10.77µg/g，总含量为34.20～83.41µg/g。结论初步拟定米炒北沙参饮片中水分、总灰分、酸不溶性灰分分别不得过7.30％、4.10％、0.30％，水溶性浸出物和醇溶性浸出物分别不得少于21.00％、18.00％，香豆素类成分的总含量分别不得少于52.03μg/g（有皮）、26.34μg/g（去皮）。所建质量标准可用于米炒北沙参的质量控制。 |
| ABSTRACT： | OBJECTIVE To establish a quality standard for rice-fired Glehnia littoralis . METHODS Appearance observation ， powder microscopic identification and thin-layer chromatography （TLC）identification were performed for the samples of rice-fired G. littoralis decoction piece. According to the relevant methods stated in 2020 edition of Chinese Pharmacopoeia （part Ⅳ），the contents of moisture ，total ash ，acid-insoluble ash ，water-soluble extract and acid-soluble extract were determined. The contents of psoralen，zanthoxylin，bergapten，imperatorin and isoimperatorin were determined by high performance liquid chromatography （HPLC）. RESULTS The rice-fired G. littoralis decoction pieces were round-like small segments ，slightly rough ，yellow（peeled） or dark yellowish brown （with peel ），special gas and slightly sweet taste. The powder was yellowish white. Under the microscope ， secretions and secretory cells ，ducts，gelatinized starch granules ，ray cells ，parenchyma cells ，etc. could be seen. TLC showed the spots developed clearly. In the chromatogram of the test sample ，there was the same blue fluorescent spot at the corresponding position of the chromatogram of isoimperatorin control sample. The moisture ，total ash ，acid-insoluble ash ，water-soluble extract and ethanol-soluble extract from 9 batches of samples were 5.82％-6.27％，3.19％-3.59％，0.21％-0.27％，24.91％-30.30％ and 20.66％ -25.83％ ，respectively. The linear range of psoralen ，zanthotoxin，bergapten，imperatorin and isoimperatorin were 0.240-2.400，0.320-3.200，0.224-2.240，0.292-2.920，0.208-2.080 µg/mL（all r＞0.999 0）. Limits of quantitation were 0.032 0， 0.030 0，0325 0，0.032 0，0.045 0 µg，respectively. Limits of detection were 0.100 8，0.089 6，0.071 5，0.090 0，0.132 0 µg， respectively. RSDs of prescision ，stability（24 h）and reprodu- cibility tests were less than 3％. Average recoveries were 100.56％ （RSD＝1.36％ ，n＝6），100.73％（RSD＝2.25％ ，n＝6）， 100.36％（RSD＝0.98％，n＝6），98.24％（RSD＝0.40％，n＝6） E-mail：853063968@qq.com and 99.40％（RSD＝0.35％，n＝6），respectively. The contents of above five components were 5.85-13.31，8.63-33.38，6.23- E-mail：shixiaofeng2005@sina.com 15.25，6.12-12.98，5.52-10.77 µg/g，respectively. The total contents were 34.20-83.47 µg/g. CONCLUSIONS It is preliminarily proposed that the moisture ，total ash and acid-insoluble ash should not exceed 7.30％，4.10％，0.30％. The water-soluble extract and ethanol-soluble extract are no less than 21.00％ and 18.00％，respectively. The total content of coumarin should not be less than 52.03 µg/g（with peel ）and 26.34 μg/g（peeled）. Established quality standard can be used for the quality control of rice-fired G. littoralis . |
| 期刊： | 2022年第33卷第08期 |
| 作者： | 王新娣，石晓峰，张晓萍，刘东彦，沈薇，范彬，马趣环 |
| AUTHORS： | WANG Xindi，SHI Xiaofeng ，ZHANG Xiaoping ，LIU Dongyan ，SHEN Wei，FAN Bin，MA Quhuan |
| 关键字： | 米炒北沙参；质量标准；显微鉴别；薄层色谱；高效液相色谱法；含量测定 |
| KEYWORDS： | rice-fired Glehnia littoralis ；quality standard ；microscopic identification ；TLC；HPLC；content determination |
| 阅读数： | 212 次 |
| 本月下载数： | 4 次 |
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