1.上海中医药大学中药研究所,中药标准化教育部重点实验室,国家中医药管理局中药新资源与质量评价重点实验室,上海中药标准化研究中心(上海 201203)
张倩,女,硕士研究生,主要从事中药化学成分分离鉴定及其质量分析研究工作
谷丽华,研究员,硕士研究生导师; E-mail: lhgu@shutcm.edu.cn
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张倩,金武燮,陆美龙,等.石菖蒲配方颗粒特征图谱及其尿苷含量测定研究[J].上海中医药杂志,2023,57(7):72-80.
ZHANG Qian,KIM Mooseob,LU Meilong,et al.Study on characteristic chromatograms and uridine content determination ofAcori Tatarinowii Rhizoma formula granules[J].Shanghai Journal of Traditional Chinese Medicine,2023,57(7):72-80.
张倩,金武燮,陆美龙,等.石菖蒲配方颗粒特征图谱及其尿苷含量测定研究[J].上海中医药杂志,2023,57(7):72-80. DOI: 10.16305/j.1007-1334.2023.2211143.
ZHANG Qian,KIM Mooseob,LU Meilong,et al.Study on characteristic chromatograms and uridine content determination ofAcori Tatarinowii Rhizoma formula granules[J].Shanghai Journal of Traditional Chinese Medicine,2023,57(7):72-80. DOI: 10.16305/j.1007-1334.2023.2211143.
目的,2,为控制石菖蒲配方颗粒内在质量,分别建立超高效液相色谱(UPLC)法整体特征图谱和高效液相色谱(HPLC)法水溶性成分特征图谱,且对核酸成分尿苷进行HPLC法含量测定。,方法,2,UPLC法整体特征图谱采用Waters ACQUITY UPLC BEH C,18, 色谱柱(2.1 mm×100 mm, 1.7 μm),以甲醇、0.1%磷酸水溶液为流动相进行梯度洗脱,流速0.4 mL/min,检测波长280 nm,柱温35 ℃,进样量1 μL;HPLC法水溶性成分特征图谱及含量测定采用SHIMADZU Shim-pack GIST C,18,-AQ色谱柱(4.6 mm×250 mm, 5 μm),以甲醇、0.1%磷酸水溶液为流动相进行梯度洗脱,流速1 mL/min,检测波长260 nm,柱温35 ℃,进样量10 μL。,结果,2,石菖蒲配方颗粒的整体性特征图谱共有9个特征峰,其中4个特征峰分别是细辛醛(峰3)、,N,-反式阿魏酰酪胺(峰4)、 ,β,-细辛醚(峰6)和,α,-细辛醚(峰9),10批样品与共有模式图的相似度在0.994~1.000之间;石菖蒲配方颗粒的水溶性特征图谱共获得8个特征峰,指认其中5个特征峰,分别为腺嘌呤(峰1)、尿苷(峰2)、腺苷(峰3)、鸟苷(峰5)和,L,-苯丙氨酸(峰7),23批样品与共有模式图的相似度在0.931~0.972之间。定量实验显示,尿苷浓度在2.086~104.300 mg/L范围内与峰面积呈现良好的线性关系(,R,2,=1.000 0),加样回收率平均值为100.16%,,RSD,值为2.02%,23批石菖蒲配方颗粒尿苷含量在0.037%~0.061%之间,配方颗粒质量稳定。,结论,2,研究所建立的两种特征图谱和含量测定方法操作简便,重复性和专属性好,可用于石菖蒲配方颗粒的质量控制。
Objective,2,To control the internal quality of Shichangpu (Acori Tatarinowii Rhizoma) formula granules, the overall characteristic chromatogram by ultra-performance liquid chromatography (UPLC) and the characteristic chromatogram of water-soluble components by high-performance liquid chromatography (HPLC) were established, and the content of uridine, a nucleic acid component, was determined by HPLC.,Methods,2,The overall UPLC characteristic chromatogram was determined on a Waters ACQUITY UPLC BEH C,18, column (2.1 mm×100 mm, 1.7 μm) with a gradient elution of methanol and 0.1% phosphoric acid aqueous solution as mobile phases at a flow rate of 0.4 mL/min, detection wavelength of 280 nm, column temperature of 35 ℃, and injection volume of 1 μL. The HPLC characteristic chromatogram of water-soluble components and content determination were performed on a SHIMADZU Shim-pack GIST C,18,-AQ column (4.6 mm×250 mm, 5 μm) with a gradient elution of methanol and 0.1% phosphoric acid aqueous solution as mobile phases at a flow rate of 1 mL/min, detection wavelength of 260 nm, column temperature of 35 ℃, and injection volume of 10 μL.,Results,2,The overall characteristic chromatogram of Acori Tatarinowii Rhizoma formula granules was established with 9 characteristic peaks, among which 4 peaks were identified as asarylaldehyde (peak 3), ,N,-,trans,-feruloyltyramine (peak 4), ,β,-asarone (peak 6), and ,α,-asarone (peak 9), with similarities of 10 bathes of samples ranging from 0.994 to 1.000. The water solubility characteristic chromatogram Acori Tatarinowii Rhizoma formula granules was established with 8 characteristic peaks, among which 5 component peaks were identified as adenine (peak 1), uridine (peak 2), adenosine (peak 3), guanosine (peak 5), and ,L,-phenylalanine (peak 7), with similarities of 23 batches of samples ranging from 0.931 and 0.972. According to the quantitative analysis, the concentration of uridine had a good linear relationship with the peak area in the linear range of 2.086 to 104.300 mg/L (,R,2,=1.000 0), the mean spiked recovery was 100.16%, the ,RSD, value was 2.02%, and the uridine content of 23 batches of Acori Tatarinowii Rhizoma formula granules ranged from 0.037% to 0.061%, showing the stable quality of the formulation granules.,Conclusion,2,The established characteristic chromatograms and content determination methods are simple, reproducible, and specific, and can be used for the quality control of Acori Tatarinowii Rhizoma formula granules.
石菖蒲配方颗粒特征图谱含量测定高效液相色谱质量标准中药研究
Shichangpu (Acori Tatarinowii Rhizoma)formula granulecharacteristic chromatogramassayHPLCquality standardtraditional Chinese herbal medicine research
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