Qiangli pipa syrup fingerprint spectrum quality control method
A quality control method, the powerful loquat dew technology, which is applied in the field of fingerprint analysis, can solve problems such as backwardness, and achieve the effect of scientific detection and stable quality
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Embodiment 1
[0031] (1) Accurately measure 25ml of the content of Qiangli loquat dew; place it in a separatory funnel, extract 4 times with water-saturated n-butanol, 25ml each time, combine the n-butanol solution, evaporate to dryness in a water bath, dissolve the residue with 50% methanol and Set the volume in a 5ml measuring bottle, shake well, filter with a 0.45 μm microporous membrane, and take the filtrate to obtain the product solution to be tested; (2) Repeat 6 times to obtain the fingerprint of the above solution to obtain 6 fingerprints , the acquisition method of fingerprint spectrum is: with 5g / L ammonium acetate aqueous solution A (adjust pH value to 7.5 with ammonia test solution) and acetonitrile B according to the mixed solution that certain volume ratio forms as mobile phase, chromatographic condition is: adopt Diamonsil C 18 Chromatographic column (150mm×4.6mm, 5μm); linear gradient elution program: within 0 to 30 minutes, the volume fraction of B in the mobile phase is 2%...
Embodiment 2
[0039] (1) Precisely measure 150ml of the content of the same batch of strong loquat dew, divide it into 6 parts, 25ml each; place them in a separatory funnel, extract 4 times with saturated n-butanol, 25ml each time, and combine n-butanol solution, evaporated to dryness in a water bath, the residue was dissolved with 50% methanol and fixed volume in a 5ml measuring bottle, shaken up, filtered with a 0.45 μm microporous membrane, and the filtrate was taken to obtain 6 parts of the product solution to be tested;
[0040] (2) Obtain the fingerprints of the above-mentioned 6 parts of product solutions to be tested, and obtain 6 fingerprints. The acquisition method is: with 5g / L ammonium acetate aqueous solution A (adjust the pH value to 7.5 with ammonia test solution) and acetonitrile B according to a certain The mixed solution of volume ratio composition is mobile phase, and chromatographic condition is: adopt Diamonsil C 18 Chromatographic column (150mm×4.6mm, 5μm); linear grad...
Embodiment 3
[0048] (1) Accurately measure 25ml of the content of Qiangli loquat dew; place it in a separatory funnel, extract 4 times with water-saturated n-butanol, 25ml each time, combine the n-butanol solution, evaporate to dryness in a water bath, dissolve the residue with 50% methanol and Set the volume in a 5ml measuring bottle, shake well, filter with a 0.45 μm microporous membrane, and take the subsequent filtrate to obtain the product solution to be tested;
[0049] (2) Place the solution of the product to be tested at room temperature for 0h, 3h, 6h, 9h, 12h, 18h, and 24h, then inject and analyze, and obtain 7 fingerprints. The results are shown in image 3 , see Table 3-1 and 3-2 for related data. Results The RSD of the retention time of each peak was less than 0.14%, and the peak area RSD of the peak with a single peak area greater than 0.5% of the total peak area was less than 1.72%. Taking the fingerprint spectrum analyzed at 0 time as a contrast, the chromatograms analyzed...
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