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@#Using high performance liquid chromatography and high resolution orbital trap mass spectrometry, a two-dimensional online desalting detection method was established to determine the structure of the impurities detected under the official testing conditions of lansoprazole enteric solution preparation, and a chromatographic method compatible with mass spectrometry was established to determine and presume the structure of the impurities that could not be separated by the the official testing method.The identification of impurity was to presume its structure according to the presence of impurity reference product, so as to investigate the difference of impurity spectrum of products from different manufacturers.The one-dimensional chromatographic conditions for the 2D online desalting method were the same as those in China Pharmacopoeia (2020) under relevant substances.Two-dimensional chromatography was performed on a Waters C18 T3 column (2.1 mm × 100 mm, 1.7 μm) with 0.1% formic acid in water-acetonitrile mobile phase and gradient elution.The chromatographic conditions for the compatible mass spectra were based on an Agilent Extend C18 (4.6 mm × 150 mm, 5 μm) column with mobile phase A: 25 mmol/L ammonium acetate and B: 25 mmol/L ammonium acetate-acetonitrile (1∶4) [pH adjusted to 6.5 with glacial acetic acid], with gradient elution. Nine impurities were detected by two-dimensional online desalting method, with 5 known impurities (A-E) and 4 unknown ones.14 impurities were detected by the compatible mass spectrometry method, with 9 unknown impurities (4 consistent with the results of two-dimensional online desalting method, and 5 newly detected).The structures and sources of the unknown impurities were deduced.The two detection methods of lansoprazole preparation by high-performance liquid chromatography-high resolution orbital trap mass spectrometry have guiding significance for quality control and process evaluation.
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@#This study was to evaluate quality consistency of domestic generic and reference preparations. Content and related substances of domestic generic preparations and reference preparation were inspected according to Chinese Pharmacopeia 2015. Then the basic solution for determining dissolution curve was established through preliminary experiment and validation for determination. The dissolution curves of domestic rifampicin capsules and reference preparation were compared in four dissolution mediums: HCl(pH 1. 2), PBS(pH 4. 0), PBS(pH 6. 8)and pure water, respectively. Results showed that the content and related substances of domestic generic and reference preparations complied with the quality standard, but impurity profile displayed that impurities in domestic generic preparations were less than those in the reference preparation, with the content of rifampin quinine being especially less. Furthermore, dissolution of domestic generic and reference preparations were compared, and their dissolution curves were not similar. It is suggested that consistency between domestic rifampicin capsules and reference preparation should be evaluated by bioequivalence test.
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@#This study aimed to isolate and prepare highly purified impurity C from doxycycline hyclate by a preparative HPLC method and to inspect the toxicity and in vitro antimicrobial activity of the impurity C of doxycycline hyclate. The solution of doxycycline hyclate treated with heat produced a solution containing 10% of impurity C which was firstly separated by the Sapphire C18(21. 2 mm×250 mm, 5 μm)column with 0. 1% acetic acid-acetonitrile(83 ∶17)as the mobile phase at 20 mL/min. Secondly, rotary evaporation of the eluted solution at the time of 8. 4 min was performed at 50 °C to remove organic solvent. Then the target product was prepared after freeze drying of evaporated solution adjusting pH to 1. 8 with formic acid. The target product was identified with ultraviolet absorbance(UV), infrared(IR), mass spectrometry(MS)and nuclear magnetic resonance(NMR), and its purity was be determined by HPLC. Meanwhile, cytotoxicity and genotoxicity in the Chinese hamster lung cells, toxicity on the development of zebrafish embryos and in vitro antimicrobial activity were compared among impurity C of doxycycline hyclate, doxycycline, metacycline and β-doxycycline. Results showed that prepared product was confirmed to be the impurity C of doxycycline hyclate. Its purity was 90. 1%, which had been the highest so far. In the cellular toxic tests and genetic toxic tests of Chinese hamster lung cells, impurity C of doxycycline hyclate, doxycycline, metacycline and β-doxycycline were somewhat toxic to Chinese hamster lung cells. Toxicity gradually decreased from doxycycline, impurity C of doxycycline hyclate, β-doxycycline to metacycline from -S9mix test results; toxicity gradually decreased from doxycycline, β-doxycycline, impurity C of doxycycline hyclate to metacycline from +S9mix test results; the aberration rate of all the tested related substances was less than 5%, and no obvious genotoxicity was found. According to test results of the development of zebrafish embryos, impurity C of doxycycline hyclate showed the strongest teratogenicity and lethality. Invitro antimicrobial tests revealed that impurity C of doxycycline hyclate had a weaker antimicrobial activity, and invitro antimicrobial activity potential of the tested compounds followed the order: metacycline, doxycycline, impurity C of doxycycline hyclate, β-doxycycline. Studies on safety and effectiveness indicated that impurity C of doxycycline hyclate belonged to toxic and ineffective impurity and need to be controlled individually in quality standard. A useful suggestion was given to revise the quality standard of doxycycline hyclate and its preparation in the current Pharmacopoeia of the People′s Republic of China.
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<p><b>OBJECTIVE</b>To analyze the occurrence feature of adverse events following immunization (AEFI) of Hib conjugate vaccine (HibCV) and to evaluate the safety of HibCV in postmarketing.</p><p><b>METHODS</b>2008-2013 HibCV AEFI data were collected through national AEFI information management system, which were downloaded in March 18, 2014.The demographic information and inoculation quantity of HibCV were from Immunization information management system in Jiangsu province. The incidence rate and 95% CI value of AEFI, common vaccine reaction and rare vaccine reaction following immunization of HibCV were calculated. The differences in the incidence rate of common vaccine reaction and rare vaccine reaction among sex, months of age, and number of injections were compared by means of (χ² tests.</p><p><b>RESULTS</b>A total of 6.16 million doses of vaccine were administered in Jiangsu province during 2008-2013, and 4 718 vaccinees reported having adverse event, for a rate of 76.60/100 000 (95% CI: 74.42/100 000-78.79/100 000). The incidence rate of common vaccine reaction and rare vaccine reaction was 71.10/100 000 (95% CI: 68.99/100 000-73.20/100 000) and 5.16/100 000 (95% CI: 4.60/100 000-5.73/100 000), respectively. The main symptoms of common vaccine reactions were fever, swelling, indurations and gastrointestinal reactions. The incidence rates of them were 40.54/100 000, 35.09/100 000, 12.94/100 000 and 0.36/100 000 in turn. The main symptoms of rare vaccine reactions were anaphylactic rashes and angioedema, the incidence rates of which were 4.77/100 000 and 0.15/100 000 respectively. 91.39% (4 002/4 379) of common vaccine reactions and 88.36% (281/318) of rare vaccine reactions happened within 1 d after vaccination. Anaphylactic shock (3 cases) and laryngeal edema (1 case) all happened within 1 d after vaccination. The incidence rate of common vaccine reactions among boys (79.72/100 000, 2 641/3 313 071) was higher than that of girls (61.07/100 000, 1 738/2 846 001) (χ² = 74.92, P < 0.001). The incidence rate of common vaccine reactions among children aged ≥ 12 month-old (86.82/100 000, 2 200/2 533 949) was higher than that among children aged 2-11 month-old (60.11/100 000, 2 179/3 625 123) (χ² = 149.79, P < 0.001). The incidence rate of common vaccine reactions in children vaccinated the first dose (78.93/100 000, 2 666/3 377 614) was higher than that in children vaccinated the second or third or fourth dose (61.59/100 000, 1 713/2 781 458) (χ² = 64.59, P < 0.001). The incidence rate of rare vaccine reactions in children vaccinated the first dose (6.69/100 000, 226/3 377 614) was higher than that in children vaccinated the second or third or fourth dose (3.31/100 000, 92/2 781 458) (χ² = 33.82, P < 0.001).</p><p><b>CONCLUSION</b>The safety of HibCV among children was relative good. However, the surveillance should still focus on the anaphylactoid reactions of anaphylactic shock and laryngeal edema after HibCV immunization.</p>
Subject(s)
Child , Female , Humans , Male , Angioedema , Bacterial Capsules , Fever , Haemophilus Infections , Haemophilus Vaccines , Haemophilus influenzae type b , Hypersensitivity , Immunization , Influenza, Human , Safety , Vaccination , Vaccines, ConjugateABSTRACT
Objective To investigate the current status of prevalence and its relative factors of non-alcoholic fatty liver disease (NAFLD) in the elderly in urban community in Ningxia province and to compare the differences in prevalence of NAFLD between Han and Hui ethnicities.Methods 1046 residents aged 55 years and over from five communities were selected.Questionnaire survey and clinical examination were conducted in all subjects.Fasting vein blood samples were collected.The serum total cholesterol,triglyceride,high density lipoprotein cholesterol,low density lipoprotein cholesterol were detected.Results There were 1043 subjects with average age of (66.41 6.65) years finishing the whole examination,including 696 (66.7％) Han and 347 (33.3％) Hui people.The total prevalence of NAFLD was 27.0％ (286/1043),and there was a significant difference in the prevalence [23.4％ (94 cases) vs.29.9％ (192 cases),x2 =5.18,P=0.023]between male and female,but no difference between Han and Hui ethnicities [28.2％ (98 cases) vs.27.0％ (188 cases) x2 =0.17,P=0.675].Logistic regression showed that age(OR=0.96,95％ CI:0.94-0.99),BMI(OR=1.31,95％ CI:1.24-1.38),TG(OR=1.71,95％ CI:1.47-1.98),central obesity (CO)(OR=5.20,95％CI:2.21-12.23) were the factors correlating with NAFLD.Conclusions The prevalence of NAFLD in Hui elderly people was is similar to that in Han elderly people.The elderly people with overweight,central obesity and high serum level of triglyceride and high level TG have higher risk for NAFLD.
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Objective: To explore the feasibility with the safety at peri-operative and early post-operative periods for left atrial appendage occlusion in patients with non-valvular atrial ifbrillation (AF). Methods: A total of 17 non-valvular AF patients with transesophageal echocardiography (TEE) and CAHDS2 evaluation who received left atrial appendage occlusion in our hospital were summarized. The effect and complications during peri-operative and 1 month post-operative periods were analyzed. Results: All 17 patients had successful operation without severe complications. There were 8 patients having small amount residual shunt by TEE examination, 2 having ecchymosis near the puncture point at peri-operative period and 3 having small amount of hydropericardium by peri-cardio ultrasound examination. At the average of 45 days follow-up study, only 3 patients had small amount residual shunt, no left atrium thrombus and hydropericardium were observed. Conclusion: Left atrial appendage occlusion has the high success rate, it is safe during peri-operative and early post-operative periods in non-valvular AF patients.
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<p><b>OBJECTIVE</b>To study the physiological and biochemical changes during storage of angelica seeds with different moisture contents.</p><p><b>METHOD</b>The dynamic changes of percentage and index of seeds germination, relative conductivity, superoxide dismutase (SOD) activity, contents of soluble sugar and protein were determined at an interval of every two months.</p><p><b>RESULT</b>Under the conditions stored in sealed paper cups at 15 degrees C for 10 months, the germination percentage of angelica seeds with 2.85% of moisture content was kept above 85%. With moisture content reducing, the increase rate of relative conductivity decreased, the down trend of SOD activity and protein content were weakened, and soluble sugar content kept stable.</p><p><b>CONCLUSION</b>In cool conditions, a modest low moisture content of seeds can be beneficial to prolong the longevity of angelica seeds, while high moisture content will accelerate the deterioration process of the seeds.</p>
Subject(s)
Angelica , Metabolism , Carbohydrates , Germination , Physiology , Plant Proteins , Metabolism , Seeds , Metabolism , Superoxide Dismutase , Metabolism , Temperature , Time Factors , Water , MetabolismABSTRACT
ObjectiveTo study electrophysiological characteristics and catheter ablation left-sided accessory pathways of Mahaim fiber.MethodsTwenty-eight patients underwent catheter ablation for Mabaim fiber and 3 patients was left-sided accessory pathways.All of them were male with 34,20,38 years old.The tachycardia history was1-5years. Electrophysiological characteristics,target sitesand electrocardiogram(ECG,12 leads) were recorded through catheter from coronary sinus(CS),high right atrium(HRA),His bundle and ablation.ResultsOne patient's ECG showed little preexcitation,the other two were normal. Atrial stimulation could be easily induced tachycardia.Their ECG showed wide QRS waves (right bundle branch block or similar right bundle branch block).The characteristics of accessory pathways were slow and anterograde decremental conduction as well as blocked by adenosine triphosphate injection.Ventricular-atrial conduction was via atrioventricular node with centripetal decreasing transmission during ventricular pacing.During tachycardia,the His bundle electrogram resulted in a V-H-A pattern,the retrograde A in His bundle was pioneer.The atriofascicular pathways of 2 patients were completely ablated respectively in left posterior lateral and before the free wall of mitral valve ring.The nodoventricular pathway of 1 patient was successfully ablated in left middle posterior lateral of mitral valve ring.ConclusionsThe left-sided accessory pathways of Mahaim fiber is an uncommon accessory pathway,which has specific electrophysiological characteristics.It is effective and safe to ablate accessory pathway with radiofrequency.
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Aim: To establish an HPLC method for the determination of secnidazole and its related substances, and to elucidate the structure of the main related substances. Methods: HPLC was performed on an Agilent C_(18) (150 mm × 4. 6 mm, 5 μm) column. The mobile phase consisted of acetonitrile and 0. 1% formic acid solution( 10 : 90). The detection wavelength was set at 320 nm and the column oven was maintained at 30 ℃. The mass spec-trometry detector was equipped with an ESI source with a temperature of 350 ℃, and set at positive ion monito-ring model The spray chamber pressure was 0. 34 MPa. The drying gas flow rate was 10 L/min. Results: Sec-nidazole was completely separated from the impurities. The calibration curve of secnidazole was linear over the range of 0. 10-1 500. 0 μg/mL with the correlation coefficient of 0. 999 9. The contents of secnidazole in the sam-ples were 100.5%, 100.3% and 100.7%, respectively, and those of the related substances were 0.463%, 0. 488% and 0.465%, respectively. The three related substances were identified by HPLC-UV-MS~n as 2-methyl-5-nitroimida-zole and the isomerides of secnidazole, respectively. Conclusion: The developed method is reliable for the quality control and determination of related substances of secnidazole.
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Measles surveillance in Jiangsu Province started in 1999 by dividing the province into two sorts of areas. The first sort of area is economic well-developed area where EPI is carried out well and measles incidence is lower. The cities of this area investigated included Suzhou, Wuxi, Changzhou and Zhenjiang. The second sort of area included 9 cities (Nanjing, Xuzhou, Liangyungang, Nantong, Huaiyin, Suqian, Yangcheng, Yangzhou and Taizhou) where all the conditions are not as good as that mentioned in the first sort of area. The surveillance system of the province reported in 1999 a total of 938 suspected measles cases in 13 cities, of which 684 were confirmed as measles. The notifiable reporting system reported 846 suspected measles cases and 684 cases were confirmed. This indicated that the surveillance system operated well. The measles epidemiological features in two sorts of areas were compared. In first sort of area, including Nanjing, the measles cases of ≥15 years old accounted for 66.3% of the total cases. In second sort of area, not including Nanjing, the measles cases of <15 years old accounted for 90.8% of the total cases, and 73.2% of them were patients <10 years old. In 1999, there were 10 measles outbreaks occurred in the province and 218 measles cases were reported which accounted for 31.7% of the confirmed measles cases reported by the provincial measles surveillance system. 9% the 10 outbreaks occurred in the second sort of area, the cases were preschool and primary school children. The results showed that progression of EPI work was uneven in two sorts of areas of Jiangsu Province.