| Senile dementia is gradually replaced diabetes as following the heart and cerebral vessels disease and malignant tumor of the elderly third largest killer, because of its irreversibility the clinical course of the disease is very difficult to patients with abnormal behavior, also brought a heavy burden to the family., ergot Lin can rapidly improve the symptoms of chronic brain function is not complete (CCI), tinnitus and dizziness symptoms improved particularly significant, sales for the world’s leading one of the central nervous system drugs. Domestic problems with ergot source, completely dependent on imported API production preparation, on the premise of active pharmaceutical ingredients with no national standard, the quality of the tablets in the standard for the serious shortage of related material control, may lead to preparation factory quality differences, increase clinical adverse reactions after use, the shelf life quality is not stable. For China’s food and drug verification research institute issued specification of ergot Lin for quality evaluation and its preparations, provide a reference for revision of the quality standards and improve in the future.Using HPLC method of ergot Lin piece of content is higher in the domestic preparation of the material to the three kinds of quantitative testing, mobile phase of acetonitrile methanol-phosphate buffer solution (potassium dihydrogen phosphate6.8g, water900ml dissolves, with triethylamine adjust pH value to7.0, diluted with water to1000ml)(30:35:35), using C18chromatographic column, under288nm wavelength detection, each impurity separating degree good, precision, accuracy, linear satisfies the requirement of drug quality standard analytical method validation guidelines, the method is simple and easy, suitable for the daily supervision to sample. While using liquid mass combination method of the three kinds of related substances for further quantitative study, using ZORBAX Eclipse Plus C182.1×50mm1.8μm chromatographic column, acetonitrile2mmol·L-1containing0.1%formic acid ammonium formate solution as mobile phase, gradient elution conditions were analyzed using positive ion mode for related substances test, to obtain a lower detection limit, better specificity, to replace the liquid chromatography (HPLC) in the near future as a means of control of related substances, for basic research. Two unknown related substances found in the process, needs further research. To accelerate factors on the part of relevant material to produce-the residues of lithium ion, ion chromatography was developed for quantitative analysis, the use of Thermo IonPac CS12A cation exchange column and IonPac CG12A protected column; CSRS suppressor, eluent for24mmol·L-1under the condition of methanesulfonic acid solution with potassium, sodium, calcium, magnesium, common metal cation degree of separation is good,This paper set up the related substances of HPLC and LC-MS/MS method and ion chromatography can be used for ergot Lin piece of quality control, method is scientific, simple and rapid, and can improve the current quality standard content, control the quality of products. The discovery of two unknown related substances for the future lay the foundation for further study, the varieties of related substances and can promote the improvement of preparation plant process itself. In this paper, the experimental research for the variety provide a basis for the revision of quality standards. |
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