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Pediatric Antipyretic Oral Liquid is one of the varieties that raises the standard by the Ministry. However, because the original quality standard is too simple, there are only identification items, no content determination items, and it is impossible to control the quality of the products. The content determination item is hereby determined by high performance liquid chromatography for the content of paeonol, an active ingredient contained in the product. The liquid chromatography method is simple in operation, good in precision, stable, and reliable in results. Since this product is a liquid preparation, this method can be directly injected, and the separation is good, and the error is reduced. Determination of paeonol in Xiaoer Antipyretic Oral Liquid by high performance liquid chromatography improves the quality of the drug and controls the quality of the finished product HPLC Vials.
1 Instruments and reagents: 1.1 Instruments: LC-10A high performance liquid chromatography HPLC (Shimadzu Corporation, Japan), SPD-10A detector, Weimaron chromatography workstation. 1.2 Test drugs: Pediatric antipyretic oral liquid and negative samples are provided by Xintian Pharmaceutical Co., Ltd., and paeonol reference substance is provided by China National Institute for the Control of Pharmaceutical and Biological Products (for content determination). Acetonitrile is chromatographically pure and water is twice double distilled water.
2 Methods and results: 2.1 chromatographic conditions: the column HPLC Vials was Sphevisorb C18 (5μm, 250mm × 5.0mm), mobile phase: acetonitrile - water (45:55), column temperature: 25 ° C, flow rate: 1ml / min, detection wavelength: 254nm . 2.2 Preparation of reference solution Take appropriate amount of paeonol reference substance, add methanol to make 0.05mg solution per 1ml, shake well, that is.
2.3 Preparation of sample solution: Take appropriate amount of this product, filter, discard the initial filtrate, and take the filtrate as the test solution.
2.4 Preparation of standard curve: precision pipetting of paeonol control solution HPLC Vials (0.0501mg/ml) 2,6,10,14,18μl injection, recording chromatogram, peak area as abscissa, injection volume (μg) as vertical The coordinates were plotted and the regression equation was calculated as: C = 5.4684 × 10-7A - 6.5334 × 10 -3 (r = 0.9998). The results showed that paeonol had a good linear relationship in the range of 0.1002μg~0.9018μg.
2.5 Precision test: 10μl of the test solution was accurately aspirated, and the injection was repeated 5 times. According to the chromatographic conditions described in the text, the chromatogram was recorded and calculated. The RSD was 0.87%, indicating good precision.
2.6 Reproducibility test: Take a sample according to the preparation method of the test solution to prepare 5 samples for the test solution, respectively accurately draw 10 μl of the test solution for injection, record the chromatogram, calculate, RSD is 1.2%, indicating good weight Present.
2.7 sample recovery rate test: using sample recovery, precision extraction of the measured content of 1ml sample, and then add paeonol reference substance (0.0501mg / ml) 1ml, according to the chromatographic conditions described in the text, calculate the recovery rate, paeonol The recovery of phenol was 100.5%, and the RSD was 1.0%, indicating that the method has a good recovery rate.
2.8 blank test: a negative sample was prepared according to the prescription ratio and production preparation method HPLC Vials. The negative solution was prepared according to the “preparation of sample solution”, 10 μl was injected, and the chromatogram was recorded. The chromatogram of the sample did not correspond to the peak of the chromatogram of the reference product. The peak indicates that the negative sample solution has no interference peak at the peak of paeonol HPLC.
2.9 Assay: 10 μl of each of the reference solution and the test solution were accurately weighed and injected into a liquid chromatograph for measurement.
3 sample determination: take all samples according to the sample solution preparation operation, respectively, draw the reference solution and the sample solution 10μl each injection, according to the above chromatographic conditions, record the chromatogram, calculate.
4 Discussion: In the preparation of the sample solution, it was concentrated and extracted with diethyl ether, evaporated to dryness, and added with methanol to make it into volume. However, because paeonol is volatile, the operation process is easy to lose, resulting in inaccurate results. The result is direct injection, the resolution is good, and there is no impurity interference at the peak of paeonol. Therefore, the product is directly injected here. The mobile phase was previously treated with methanol-water-ice [CM(14]acetic acid (55:45:2), methanol-water (55:45), acetonitrile-water-glacial acetic acid 45:55:0.2), acetonitrile-water ( 43:57) The mobile phase was tested. When the other conditions were the same, the separation effect of acetonitrile-water-glacial acetic acid (45:55:0.2) and acetonitrile-water (45:55) was better, but Acid has a certain damage to the column, resulting in a shortened service life. Therefore, acetonitrile-water (45:55) is selected as the mobile phase. The experimental results show that under this chromatographic condition, the content of paeonol in Xiaoer Jiere Oral Liquid is determined by HPLC. The method is simple, rapid and reproducible.
This is the end of the introduction of Determination of paeonol in Xiaoer Jiere Oral Liquid by HPLC. I hope it can help you.
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