Method for detecting amino acid component in Xiasangju preparation
A technology of amino acids and mulberry chrysanthemum, which is applied in the preparation of test samples, measuring device, material separation, etc., can solve the problem of difficulty in comprehensively characterizing the physical and chemical characteristics of compound mulberry chrysanthemum preparations.
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Embodiment 1
[0055] Example 1 Detection of fingerprints of amino acid components in Xiasangju sugar-containing granules
[0056] 1. Instruments and reagents
[0057] 1.1 Instruments Waters2695 high performance liquid chromatography, Waters 2475 (fluorescence detector), Empower chromatography workstation. Swiss Mettler company AE-200 electronic analytical balance.
[0058] 1.2 Reagent Derivative agent: 6-amino acid quinoline-N-hydroxysuccinimidyl-carbamate (abbreviated as AQC), amino acid reference substance: AminoAcid stadard H (Waters Company); acetonitrile (chromatographically pure), secondary heavy Distilled water, sodium acetate (analytical pure), triethylamine (analytical pure)
[0059] 2. High performance liquid chromatography
[0060]
mobile phase
time
flow
mL.min -1
A
Sodium acetate buffer mL
B
Acetonitrile solution mL
1
2
0
0.5
1
1
100
100
0
0
3
1
1
...
Embodiment 2
[0066] Example 2 Detection of fingerprints of amino acid components in 10 batches of Xiasangju sugar-containing granules
[0067] Get 10 batches of Xia Sangju granules, detect according to the conditions of Example 1, and obtain the amino acid HPLC collection of samples of 10 batches of samples, as figure 2 As shown, by comparing 10 batches of HPLC chromatograms, the similarity evaluation is carried out to determine its characteristic common peak:
[0068] There are 12 common peaks in the fingerprint spectrum. Now the retention time of the spectrum, the average value of the peak area and the RSD value are summarized, as follows:
[0069] Peak No. 1 is aspartic acid, the average retention time RT is 19.54min, the RSD is 0.05%, the peak area is 785808, the RSD is 25.04%, accounting for 1.58% of the total peak area.
[0070] The No. 2 peak is serine, the average retention time RT is 20.45min, the RSD is 0.05%, the peak area is 721818, the RSD is 33.86%, accounting for 1.46% of ...
Embodiment 3
[0088] Example 3 Method for Determination of Fingerprint of Amino Acid Components of Guangzhou Xingqun Xia Sangju Sugar-Containing Granules
[0089] (b) Preparation of the test solution: Accurately weigh 1.0 g of Xia Sangju granules produced by Guangzhou Xingqun (Pharmaceutical) Co., Ltd., put in a 10mL volumetric flask, add water to dissolve to the mark, shake well, and filter with an ultra-microporous membrane , take 10uL filtrate to the derivation tube, add 170uL boric acid buffer, and add 20uL concentration of 0.5% 6-aminoquinolyl-N-hydroxysuccinimidyl-carbamate in acetonitrile solution, vortex mix for 15 In seconds, the sample tube is sealed, placed in a 50°C oven, heated for 20 minutes, and then allowed to cool.
[0090](c) Chromatographic conditions: the chromatographic column is octadecylsilane bonded silica gel as a filler; gradient elution is adopted, and the mobile phase is a mixture of 0.05mol / L sodium acetate buffer (phase A) with a pH of 5.05 and 60% acetonitrile...
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