A method for determining the content of trace components in traditional Chinese medicine preparations
A method of determination, a trace technology, applied in the field of analytical chemistry
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Embodiment 1
[0074] Example 1 Establishment and Analysis of Danshen Injection Control Fingerprint
[0075] 1. Instruments and reagents
[0076] High-performance liquid chromatography system: Agilent 1100 Agilent Technologies, USA (configured with vacuum degasser, autosampler, quaternary pump, VWD G1314A, DAD G1315B; Agilent ChemStation A 10.02 chromatographic workstation).
[0077] Danshensu sodium reference substance, protocatechuic acid reference substance, and protocatechualdehyde reference substance were all purchased from China Institute for the Control of Pharmaceutical and Biological Products, rosmarinic acid reference substance, shikoninic acid reference substance, salvianolic acid B reference substance, caffeic acid The reference substance and the isoferulic acid reference substance were purchased from Shanghai Yousi Biotechnology Co., Ltd., and the salvianolic acid D reference substance was isolated from Salvia miltiorrhiza (self-made, with a purity of about 70%); phosphoric acid...
Embodiment 2
[0103] The establishment of embodiment 2 reference standard curve
[0104] 1. The apparatus and reagents are the same as in Example 1.
[0105] 2. Chromatographic conditions and system adaptability test
[0106] (1) The chromatographic conditions are the same as in Example 1.
[0107] (2) System adaptability test
[0108] Under the selected chromatographic conditions, the nine main phenolic acids, danshensu, protocatechuic acid, protocatechuic aldehyde, caffeic acid, isoferulic acid, salvianolic acid D, rosmarinic acid, shikonic acid and salvianolic acid The phenolic acid B has achieved baseline separation, the separation degree is greater than 1.5, the theoretical plate number of the chromatographic peak is not less than 30,000, and the symmetry factor is between 0.9-1.1.
[0109] Preparation of reference solution
[0110] Due to the large differences in the content and solubility of several main phenolic acid components in the sample, the components with similar content ...
Embodiment 3
[0188] The establishment of the standard curve of embodiment 3 reference substance
[0189] 1. Instruments and reagents
[0190] High-performance liquid chromatography system: Agilent 1100 Agilent Technologies, USA (configured with vacuum degasser, autosampler, quaternary pump, VWD G1314A, DAD G1315B; Agilent ChemStation A 10.02 chromatographic workstation).
[0191] Since salvianolic acid D is extremely unstable after purification, it is impossible to buy a reference substance that can be used for qualitative and quantitative analysis, so it is isolated from Danshen with a purity of about 70% (HPLC, peak area normalization method); phosphoric acid (85 %), formic acid (96%), and acetic acid were purchased from Tedia (USA), methanol and acetonitrile were purchased from Burdick & Jackson (Honeywell, USA), and water was prepared by Mili-Q ultrapure water apparatus.
[0192] 2. The chromatographic conditions are the same as in Example 1.
[0193] 3. Preparation of reference solu...
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