Papers Category:Medicine Papers
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Post Time:2013-1-26 10:01:00
Abstract: Objective To establish the method for the determination of paeoniflorin Xie Li Xiao Capsule method column: Kromasil C18 column (4.
6 mm × 250 mm, 5 μm, mobile phase: methanol-0.1% phosphoric acid solution (25:75, detection wavelength: 230 nm, flow rate: 1.0 mL · min-1 results paeoniflorin 0.484 ~ 2.422 μg (r = 0.999 9 linearity in the range of a good relationship, the regression equation is Y = 190 9276.923 1X - 4 265.72 (r = 0.999 9 ), average recoveries were 99.67% (RSD = 2.13% Conclusion The method is accurate and reliable, reproducible, and can be used for the paeoniflorin quality control Xie Li Xiao Capsule.
Keywords: Xie Li Xiao Capsule, paeoniflorin, HPLC
Xie Li Xiao Capsule wine Coptis, wine white peony root, prepared from 12 betel nut, Alisma, licorice, herbs processing, heat dampness, the effect of gas pain , used clinically in the large intestine damp heat caused by abdominal pain, diarrhea, poor stool, diarrhea sepsis embolism effect significantly the original standard content determination of the Coptis berberine component preparations, while the white peony nourishing yin, priorities and prescription to the drug that paeoniflorin the white peony active ingredients In the paeoniflorin preparations for the content determination, provide some reference for the perfect Xie Li Xiao Capsule quality control.
1 instrument and reagent
1.1 Instrument Agilent1100 high performance liquid chromatograph, a UV1100 UV spectrophotometer (Shanghai Tian Mei Scientific Instrument Co., Ltd., KQ-250 type ultrasonic cleaning device (Kunshan Ultrasonic Instrument Co., Ltd., AB135-S electronic balance (Mettler, Switzerland - Tropsch profitable company
1.2 reagent paeoniflorin reference substance (110736-200424 purchased from China Pharmaceutical and Biological Products, Xie Li Xiao Capsule (Yunnan Baiyao Group Co., Ltd. purchased from Qingdao Guofeng pharmacies, methanol, phosphate chromatography pure water is purified water other reagents were of analytical grade.
2 Methods and Results
2.1 Chromatographic conditions Column: Kromasil C18 column (4.6 mm × 250 mm, 5 μm, mobile phase: methanol-0.1% phosphoric acid (25 ︰ 75, the detection wavelength: at 230 nm, flow rate: 1.0 mL · min-1. Theoretical plate number paeoniflorin peak should not be less than 3000.
2.2 solution preparation
2.2.1 The reference solution take paeoniflorin reference substance, accurately weighed, dissolved in methanol, and made every 1 mL solution containing 120μg derived.
2.2.2 for the test solution to take the contents of this product, small study, taking about 0.5 g, accurately weighed, set conical flask precision of methanol was added 50 mL, said that given the weight, ultrasound treatment (power of 300 W, frequency for 50 kHz30 minutes, let cool, and then said that given the weight of methanol to complement the weight loss, shake, filtration, the precise amount of filtrate added 10 mL, evaporated to dryness, the residue 10ml water to dissolve, n-butanol saturated with water shaking extracted four times, each 20ml, combined n-butanol solution, water bath and evaporated to dryness, the residue dissolved in methanol and transferred to a 10ml volumetric flask, add methanol to the mark, shake, filtration, that is, too.
2.2.3 The negative control solution to take the rest of the Smell than white peony obtained free of white peony blank preparation, according to the method for the preparation of the test solution preparation, ie.
2.3 methodological study
2.3.1 specificity test precision draw the reference solution for 10 μL each of the test solution and the negative control solution was measured at 2.1 under chromatographic conditions. Paeoniflorin peak in the results of the test to achieve baseline separation and retention time consistent with the reference standard, negative control solution at the same retention time no absorption peak, indicating that the determination of non-interference of the rest of the Smell of paeoniflorin, the results shown in Figure 1.
Figure 1 paeoniflorin reference substance (A, the test (negative control (CHPLC Figure
2.3.2 linear relationship between the study take paeoniflorin reference substance, accurately weighed, add methanol produced per 1ml containing 242.2μg the solution, the precise amount of 2,4,6,8,10 ml, respectively set 10ml volumetric flask, add methanol to the mark, shake, measured as 2.1 under chromatographic conditions. paeoniflorin injection volume abscissa (X, corresponding to the peak area of the vertical axis (Y standard curve, the regression equation: Y = 190 9276.923 1X - 4 265.72, r = 0.999 9. paeoniflorin injection volume, respectively, 0.484 4 ~~ 2.422 0μg range a good linear relationship.
2.3.3 precision test precision drawing 2.2.1 under the reference solution, measured 2.1 under chromatographic conditions, repeated measurements, the injection volume was 10 μL. The results the paeoniflorin area RSD were 1.41% (n = 6, indicating good precision instrument.
2.3.4 stability test taken above the test solution, respectively, in the preparation of 1,3,5,7,9,12 h Determination of Paeoniflorin peak area, the injection volume was 10 μL results paeoniflorin peak area RSD were 0.96% (n = 6,, that has a good stability of the test solution within 12h.
2.3.5 Repeatability test the same batch of Xie Li Xiao Capsule (batch number 20101004 contents, 6, respectively, below the legal system 2.2.2 was the test solution, according to 2.1 under chromatographic conditions were measured injection amount of 10 μL. Results paeoniflorin average content preparation were 12.358 3 mg / g, RSD 1.69% (n = 6, shows the determination of method reproducibility than ideal. Links to free papers Download Center http://eng.hi138.com
2.3.6 sample recovery test take known content Xie Li Xiao Capsule (batch number 20100401, paeoniflorin 12.358 3 mg / g contents of 6 parts, each about 0.25g, accurately weighed, respectively, adding precision paeoniflorin reference solution (.1205 mg / mL and 25 mL of methanol each, said that given the weight of the rest at 2.2.2 under way operation, prepared for the test solution measured according to 2.1 under the chromatographic conditions, injection volume 10 μL calculated recoveries, and the results are shown in Table 1. Table 1 sample recovery test results (n = 6
2.4 Sample Determination of three batches of samples by the legal system in the preparation of the test solution for the test solution, measured at 2.1 under chromatographic conditions, each batch of samples was measured three parts, the results in Table 2.
Table 2 Sample assay results (n = 3
3 Discussion 3.1 In addition to the test preparation method to select the preparation of this study for the test screening, methanol solution directly ultrasonic treatment, injection determination of impurities serious interference paeoniflorin peak separation is not ideal, and then n-butanol extraction hybrid process , the results for the test solution paeoniflorin peak separation is good.
3.2 mobile phase preferred in this study Reference the Pharmacopeia and related literature [3,4] determination of paeoniflorin on the mobile phase of the screening, the final selection of methanol - phosphate (25:75 system, this system can effectively reduce the paeoniflorin tail good chromatographic peak shape and retention time is moderate.
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 Zhu Ming, Hu Mei Su Xue winter, such as high performance liquid chromatographic determination of the content of the the Fubao particles paeoniflorin [J]. The Chinese pharmaceutical standards; 2001,2:112-114. Posted in the free papers Download Center http://eng.hi138.com