| Sanhuang dropping pill is composed of Rhubarb, Scutellaria baicalensis georgi extract, berberine hydrochloride, which is a new type of preparation using the technical of solid dispersion. At present, the development study of it is less. However, Sanhuang tablet as one of the varieties of traditional Chinese medicine. Formula of research, quality standards and other aspects of research in it are relatively full. Due to the tablet has some shortcomings as slow dissolution rate, bioavailability is not higher, production process complicated and has long cycle. Therefore, the research is turned it into a quick-acting solid preparation Sanhuang dropping pill which is based on the composition of tablets formula and using the modern new preparation technique. We studied the optimum preparation process for Sanhuang dropping pill, which is used the orthogonal design. The high performance liquid chromatography(HPLC) method of determining its main effective component content in dropping pill is established. At the same time, we established the HPLC fingerprint of traditional Chinese medicines Sanhuang dropping pills.Objects: To improve formulation of Sanhuang tablet and provide clinical taking convenient, effective rapid preparation, orthogonal design is used to establish the optimum preparation process for Sanhuang dropping pill; In order to ensure the quality of Sanhuang dropping pill, in combination with production practice, we develop the HPLC for determination of the content of five anthraquinones constituents in rhubarb, baicalin and berberine hydrochloride. To analysis the main ingredients of the preparation from the overall and provide more comprehensive and scientific basis for effectively controlling the quality of Sanhuang dropping pill, we established the HPLC fingerprint of Sanhuang dropping pills.Methods: 1 The optimum preparation process of solid dispersions Sanhuang Dropping Pill: orthogonal design was performed to select drugs and ratio of matrix, the material liquid temperature, substrate, and kinds of coolants. The comprehensive score of appearance quality(roundness, hardness, colour and lustre, trailing) and pill weight variation for index to determine the optimum preparation process of Sanhuang Dropping Pill. 2 The method of determining the contents of five anthraquinones in Sanhuang Dropping Pill: Using Diamonsil C18(250 mm × 4.6 mm, 5μm), the mobile phase consisted of water containing Methanol-0.23% phosphoric acid solution(V:V=85:15). The flow rate was 1.0ml·min-1 and detection wavelength was 440 nm. Column temperature was room temperature. 3 The method of determining the contents of baicalin: Using Diamonsil C18(250 mm × 4.6 mm, 5μm) column with a mobile phase of phosphate-0.25% acetonitrile(V:V=30:70). The flow rate was 1.0ml·min-1 and detection wavelength was 270 nm. Column tem-perature was room temperature. 4 The method of determining the contents of berberine hydrochloride: Using Diamonsil C18(250 mm × 4.6 mm, 5 μm) column with a mobile phase of acetonitrile- water(1:1)(per 1000 ml adding potassium dihydrogen phosphate 3.4 g and 1.7 g, sodium dodecyl sulfate). The flow rate was 1.0ml·min-1 and detection wavelength was 265 nm. Column tem-perature was room temperature. 5 The establishment of A solid dispersions Sanhuang Dropping pill fingerprints: Using Diamonsil C18(250 mm × 4.6 mm, 5μm) column, mobile phase A was acetonitrile and B was water, gradient elution, elution program was 0 ~ 10 min, A was 5% ~ 95%. 10 ~ 15 min, A was 10% ~ 25%; 15 ~ 30 min, A was 25% ~ 30%; 30 ~ 50 min, A was 30% ~ 40%; 50 ~ 60 min, A was 40% ~ 45%; 60 ~ 70 min, A was 45%; 70 ~ 80 min, A was 45% ~ 50%, 80 ~ 90 min, A was 50% ~ 70%, 90 ~ 100 min, A was 70% ~ 95%, 100 ~ 110 min, A was 95% ~ 5%, 110 ~ 130 min, A was 5%. Flow rate was 0.8 ml·min- 1, detection wavelength was 254 nm, column temperature was 30℃.Results: 1 The optimum preparation process of Sanhuang Dropping Pill: dripping temperature was 90℃, the substrate for PEG4000: PEG6000 = 1:1, drugs and substrate ratio of 1:1, liquid paraffin as coolant. 2 The method of determining the contents of five anthraquinones in Sanhuang Dropping Pill: The method had good line relationship within the ranges of 0.070~0.700μg(r=0.9999, n=7), 0.646~6.460μg(r=0.9999, n=7), 0.130~1.300μg(r=0.9999, n=7), 0.150~1.500μg(r=1.0000, n=7) and 0.074~0.740μg(r=1.0000, n=7). The average recovery rate were 100.56%, 97.51%, 99.29%, 100.72%, 99.77%(RSD<3%, n=9). 3 The method of determining the contents of baicalin: The linear range of baicalin was from 0.13625μg to 0.68125μg(r = 0.9992, n = 7), the average recovery rate was 100.66%, RSD was 1.36%(n = 9). 4 The method of determining the contents of berberine hydrochloride: The linear range of berberine hydrochloride was from 0.034μg to 0.238μg(r = 0.9998, n = 7), the average recovery rate was 100.17%, RSD was 1.81%(n = 9). 5 The establishment of A solid dispersions Sanhuang Dropping pill fingerprints: establish Chinese medicine fingerprint of Sanhuang drop pills, chromatographic peak of berberine hydrochloride as reference, with a total of 15, 10 batches of sample, sample similarity were greater than 0.96.Conclusions: The best molding process which is screened by the orthogonal experiment reasonable, stable and feasible, the method is suitable for the requirement of pharmacopoeia. Content determination method is simple, accurate, specific, can be used for quality control of Sanhuang dropping pills. The establishment of the fingerprint controls the overall characteristics of Sanhuang dropping pill, it provided new basis for quality control. |
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