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1.
建立匹多莫德光学异构体检查的手性固定相HPLC法,为本品的质量控制提供有效的分析方法。色谱条件为CHIRALPAK?IA柱(250 mm×4.6 mm,5 μm),流动相为甲基叔丁基醚-乙腈-三氟乙酸(35∶65∶0.2),柱温25 ℃,流速为1.0 mL/min,检测波长为210 nm。在建立的色谱条件下,匹多莫德与其对映异构体可完全分离。本方法可用于匹多莫德原料中对映异构体的检测。 相似文献
2.
建立恩替卡韦5个光学异构体的高效液相色谱拆分方法。采用Chiralpak AD-H手性柱(250 mm×4.6 mm,5 μm)在正相条件下进行同时拆分,流动相为正己烷-异丙醇-乙醇-二乙胺(70∶6∶24∶0.1),流速为0.5 mL/min,检测波长为254 nm,柱温为30℃。色谱条件的优化过程中,考察了流动相组成及比例、酸碱添加剂、流速、柱温等因素对恩替卡韦异构体分离的影响。在所建立的条件下,恩替卡韦5个光学异构体分离良好,分离度依次为1.923,4.498,4.573和2.143。该方法简单快速、重复性好,适用于恩替卡韦原料药的光学异构体检查。 相似文献
3.
张根元 《中国药科大学学报》2007,38(6):527-529
目的:建立高效液相色谱法检查米格列奈对映异构体限量的方法。方法:采用Sumichiral OA-3300(4 mm×250mm,5μm)为手性色谱柱,以正己烷-氯仿-甲醇-三氟醋酸(50∶48∶2∶0.5)为流动相,检测波长为259 nm,流速为1 mL/min。结果:米格列奈与对映异构体达到了较好的分离,其分离度为1.9,对映异构体的最小检出量为30 ng;对映异构体峰面积与浓度线性关系良好,回归方程为A=2.593 4×103c+2.672×102(r=0.999 7,n=5)。结论:该法快速、准确,可用于米格列奈对映异构体的检查与控制。 相似文献
4.
目的:建立西酞普兰对映异构体的拆分方法。方法:采用α1-酸性糖蛋白(AGP)手性柱固定相,考察了流动相组成、pH值、流速、柱温、有机改性剂对拆分的影响,优化后色谱条件为Chrom Tech CHIRAL-AGP柱(150 mm×4.0 mm,5μm),流动相为50 mmol/L醋酸铵缓冲液(乙酸调节pH至4.3),流速0.8 mL/min,检测波长240 nm,柱温25℃。结果:西酞普兰对映异构体保留时间分别为6.8和8.4 min,能够达到基线分离。结论:缓冲盐浓度和pH值是影响对映体分离的重要因素,同时可以在一定范围内调节流速和柱温来提高柱效,改善分离。 相似文献
5.
目的:建立高效液相色谱手性固定相法拆分联萘酚对映体的新方法。方法:采用正相高效液相色谱法,CHIRALPAKIC柱(250mm×4.6mm,5μm)对联苯酚对映体进行拆分,流动相为正己烷∶异丙醇(60∶40~95∶5,V∶V)和正己烷∶无水乙醇(60∶40~95∶5,V∶V);柱温15~35℃,流速0.4~1.0mL/min,紫外检测波长254nm。根据拆分结果确定最佳色谱条件。结果:手性分离的最佳色谱条件为正己烷∶无水乙醇=80∶20(V∶V),流速0.8mL/min,柱温25℃,联萘酚对映体在6min内分离度达到2.43。结论:CHIRALPAKIC柱可以快速、高效地拆分联萘酚对映体,该方法可用于联萘酚的分离及其在不对称合成中光学纯度的快速检测。 相似文献
6.
目的建立HPLC直接分离包甲素类似物对映体的方法.方法在正相条件下,使用CHIRALPAKAD分析柱,考察了流动相的组成、流速、柱温对对映体拆分的影响;应用不同体积比的正已烷、异丙醇、二乙胺为流动相,不同的流速,对4个包甲素类似物(Ⅰ、Ⅱ、Ⅲ、Ⅳ)外消旋体分别进行了手性分离.结果得到较佳拆分色谱条件,4个包甲素类似物都能实现对映异构体的基线分离.结论此方法适用于包甲素类似物的光学纯度分析. 相似文献
7.
目的建立罗通定与其右旋对映体的HPLC手性分离方法。方法采用手性色谱柱CD-PH(250 mm×4.6 mm,5μm),观察了有机改性剂选择、离子强度、pH值、流速和柱温等对分离的影响。推荐的色谱条件为:乙醇-1.0 mol/L高氯酸钠(用磷酸调pH 3.7)(55∶45)为流动相,流速为0.15 mL/m in,柱温50℃,检测波长为280 nm。结果在本条件下,罗通定与其对映体有较好的分离,分离度达到1.45,右旋对映体检测限为100 ng。结论本方法简便、准确、快捷,可用于罗通定药物的光学纯度鉴定,在较高水平上控制罗通定口腔崩解片的质量。 相似文献
8.
HPLC法直接拆分包甲素类似物对映异构体 总被引:1,自引:0,他引:1
目的 建立HPLC直接分离包甲素类似物对映体的方法。方法 在正相条件下,使用CHIRALPAK AD分析柱,考察了流动相的组成、流速、柱温对对映体拆分的影响;应用不同体积比的正已烷、异丙醇、二乙胺为流动相,不同的流速,对4个包甲素类似物(Ⅰ、Ⅱ、Ⅲ、Ⅳ)外消旋体分别进行了手性分离。结果 得到较佳拆分色谱条件,4个包甲素类似物都能实现对映异构体的基线分离。结论 此方法适用于包甲素类似物的光学纯度分析。 相似文献
9.
目的采用磺丁基醚-β-环糊精(SBE-β-CD)作为流动相添加剂,建立反相色谱法分离尼莫地平对映体的方法。考察了环糊精的种类、浓度、有机改性剂的种类和浓度、pH值、柱温、流速等因素对对映体分离的影响。方法采用HypersilBDSC8色谱柱(150 mm×4.6 mm,5μm);流动相为水(pH2.5,含25mmol·L~(-1)SBE-β-CD)-乙腈(58:42,V/V);流速0.8 ml·min~(-1);检测波长为235nm;进样量为20μl;柱温20℃。结果在优化的色谱条件下,尼莫地平对映体达到完全分离,分离度R为1.6,分离因子α为1.1。结论该方法操作简单,比手性固定相法更经济适用。并拓展了SBE-β-CD在HPLC中作为手性流动相添加剂拆分对映体的应用。 相似文献
10.
目的:建立手性固定相(CSP)正相高效液相色谱法分离细胞裂解液中氟伐他汀对映体的分析方法。方法:采用直链淀粉-三[3,5-二甲基氨基甲酸酯]衍生物(Chiralpak AD)手性色谱柱(4.6 mm×250 mm),流动相:正己烷-无水乙醇-三氟乙酸(90∶10∶0.1),流速0.5 ml/min,检测波长:239 nm。结果:在建立的手性分离方法下,氟伐他汀消旋体在20μmol/L~300μmol/L浓度范围内线性关系良好,两个对映异构体的相关系数r2分别为0.9993、0.9997,方法回收率为(99.4±0.8)%,日内、日间精密度(RSD)均小于10%。结论:建立的正相手性固定相高效液相色谱法分离和测定细胞裂解液中氟伐他汀对映体的方法准确、可靠,可用于体外细胞模型中氟伐他汀的立体选择性研究。 相似文献
11.
Objective: To evaluatel the value of D-dimers in patients with acute aortic dissection (AAD). Methods: This study consisted of 16 patients with AAD and 27 non-AAD patients. Serum D-dimets were measured by Sta-Liatest D-DI immunoturbidimetric assay. Results: D-dimer level was higher (P < 0.001) in patients with AAD(7.91 ± 5.52 μg/ml) than that in non- AAD group(1.57±1.24 μg/ml). D-dimer was positive (>0.4 μg/ml) in all patients with AAD and in 10 control group patients (37%). Among patients with acute AAD, D-dimers tended to be higher in Stanford A than in Stanford B (8.67 ± 4.31 μg/ml vs. 3.24±1.27 μg/ml, P <0.01). D-dimer values tended to be higher in more extended disease(3.84 ± 1.65 μg/ml, 8.57 ± 3.58 μg/ml and 11.87 ± 5.69 μg/ml in thoracic aorta, thoracic and abdominal aorta, thoracic and abdominal aorta and iliacal arteries, respectively, P < 0.05 for both 8.57 ± 3.58 and 11.87 ± 5.69 vs. 3.84 ± 1.65 ). Including the control group into the analysis, we found a sensitivity of 100%, a negative predictive value of 100%, and a specificity of 66% and a positive predictive value of 64% for D-dimer in diagnosis of AAD in our patients with suspected AAD. Conclusion: D-dimer was elevated in patients with AAD. A negative D-dimer test result could be useful in excluding AAD. 相似文献
12.
Jiageng Zhu Jun Li Ruipeng Ji Jianghao Su Mingshun Shen Zhigang Cao 《南京医科大学学报(自然科学版)》2007,21(2):125-128
Objective: To set up a simple and reliable rat model of combined liver-kidney transplantation. Methods: SD rats served as both donors and recipients. 4℃ sodium lactate Ringer's was infused from portal veins to donated livers,and from abdominal aorta to donated kidneys, respectively. Anastomosis of the portal vein and the inferior vena cava (IVC) inferior to the right kidney between the graft and the recipient was performed by a double cuff method, then the superior hepatic vena cava with suture. A patch of donated renal artery was anastomosed to the recipient abdominal aorta. The urethra and bile duct were reconstructed with a simple inside bracket. Results: Among 65 cases of combined liver-kidney transplantation, the success rate in the late 40 cases was 77.5%. The function of the grafted liver and kidney remained normal. Conclusion: This rat model of combined liver-kidney transplantation can be established in common laboratory conditions with high success rate and meet the needs of renal transplantation experiment. 相似文献
13.
Tao Ye * Zhi-quan Liu Jian-jun Mu Xi-han Fu Jun Yang Bao-lin Gao and Xiao-hong Zhang Department of Cardiology First Hospital of Xi'an Jiaotong University Xi'an Hanzhong Cardiovascular Institute Hanzhong 《中国医学科学杂志(英文版)》2004,19(4):248-251
Objective To observe blood pressure change with age in salt-sensitive teenagers whose salt sensitivity were determined by repeated testing.Methods Salt sensitivity was determined through intravenous infusion of normal saline combined with volume-depletion by oral diuretic furosemide in 55 teenagers. After five years, salt sensitivity was re-examined and subject blood pressure was followed up. Blood pressure changes in salt-sensitive teenagers were compared to that of non-salt sensitive teenagers over five years.Results After 5 years, the repetition rate of salt sensitivity determined by intravenous saline loading is 92.7%. In teenagers with salt sensitivity on the baseline, both the systolic blood pressure increments and increment rates were much higher than non-salt sensitive teenagers (12.7±12.1 mmHg vs. 2.8±5.2 mmHg, P< 0.01; 12.2%± 12.0% vs. 2.5% ±4.4%, P< 0.001,respectively). There was a similar trend for diastolic blood pressure (8.4 ± 6.4 mmHg vs. 3.7 ± 6.4 mmHg, P = 0.052; 13.2% ±10.6 % vs. 6.8%± 10.1%, P = 0.053, respectively).Conclusions Salt sensitivity determined by intravenous saline loading showed good reproducibility. Blood pressure increments with age were much higher in salt-sensitive teenagers than non-salt sensitive teenagers, especially in terms of systolic blood pressure. 相似文献
14.
目的:评价使用安心颗粒对急诊经皮冠状动脉介入术(PPCI)术后生活质量的影响.方法:将160例接受PPCI的急性ST段抬高型心肌梗死患者随机分为安心颗粒组(术前顿服安心颗粒8.8g,术后安心颗粒4.4 g/次,每日2次)和对照组(仅接受基础药物治疗).所有患者均服用阿司匹林、氯吡格雷和阿托伐他汀.分别在入院时、出院前1d、出院后180 d时,应用心肌梗死多维度量表(MIDAS)、中文版SF-36评价量表对患者生活质量评分.并观察术后30 d以内的出血并发症、血小板减少症发生情况.结果:入院时和出院前1d,两组患者的心肌梗死MIDAS、SF-36量表评分比较无差异(P>0.05);出院后180 d时,与对照组比较,安心颗粒组MIDAS、SF-36评分明显减低(P<0.05);组内与入院时比较,两组出院前1d、出院后180 d时,MIDAS、SF-36评分均降低(P<0.05).两组患者在随访期间均无大量出血、少量出血、重度和极重度血小板减少症发生,安心颗粒组有4例、对照组有7例发生不明显出血(P>0.05).两组发生轻度血小板减少症的患者数比较无差异(P>0.05).结论:PPCI使用安心颗粒,能改善急性ST段抬高型心肌梗死患者的生活质量,且不增加出血风险. 相似文献
15.
Jingming Zhu Ningning Hui Xiuhong Jiang Huaxing Zhang Chengzhang Fu 《南京医科大学学报(自然科学版)》2007,21(6):386-389
Objective:To investigate the influences of urapidil and nicardipine on rabbit sinus function,atrio-ventricular node function and hemodynamics.Methods:Thirty-two Angora's rabbits were selected and randomly divided into four groups.U1 group:urapidil 0.25 mg/kg;U2 group:urapidil 0.5 mg/kg;N1 group:nicardipine 10 μg/kg;N2 group:nicardipine 20 μg/kg.All these medicine were administrated within 30 seconds.Measurements were taken before and after the administration of urapidil or nicardipine for the following data:mean blood pressure(MAP),heart rate(HR),sino-atrial conduction time(SACT),maximal sinoatrial recovery time(SNRTmax)corrected sinus node recovery time(CSNRT),index of sinus node recovery time(SNRTI),Wenckebach A-V conduction frequency (WB),and P-R interval.Results:Significant MAP and HR changes were identified in all of the four groups before and after administration of both urapidil and nicardipine.No significant changes could be found in the rest of the parameters.Intergroup analysis showed that SACT and CSNRT of N1 and N2 groups were shorter than those of the U2 group(P<0.01);the MAP decreased(P<0.01)and the HR increased drastically(P<0.01).Conclusions:Neither urapidil(0.25 mg/kg,0.5 mg/kg)nor nicardipine(10μg/kg,20μg/kg)has any significant influence on rabbit sinus function or rabbit atrio-ventricular node function.Nicardipine could be a better choice than urapidil for parafunctional sinus node patients. 相似文献
16.
Objective:To investigate the gene expression of osteoprotegerin(OPG) and osteoclast differentiation factor(ODF) in the bone tissue of patients with hip fracture due to osteoporosis. Methods:OPGmRNA and ODFmRNA in the bone tissue in 50 cases of osteoporosis sufferers(over 50 years old) with hip fracture(Observer Group) and 30 cases of hip facture sufferers with no osteoporosis(Control group) were analyzed with the Semi-Quantitative RT-PCR method. Results:The mRNA expressed of ODF, OPG were both high in the patients with hip fracture. In the control group, the expression of OPG mRNA was observed, while the expression of ODF mRNA was very slight. Conclusion:Aged patients contained all signals including OPG, ODF that are essential for inducing osteoclastogenesis and promoting bone resorption. 相似文献
17.
Scientific principles and rigorous processes should be followed in developing clinical guidelines for therapeutic interventions of integrative medicine
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A clinical guideline for the therapeutic interventions of integrative medicine may be defined as a written document which states a series of recommendations on therapeutic interventions of integrative medicine for a special disease or condition. The guideline may provide assistance to medical professionals in making clinical decisions aimed at improving the clinical outcome of patients and reducing the costs of medical care(~'4~. Recommendations issued by a guideline should be based on the best available evidence in both Western and Chinese medicine. For fulfilling this purpose, the development of clinical guidelines for therapeutic interventions in the field of integrative medicine should follow scientific principles and undergo a rigorous processes. 相似文献
18.
Objective:To probe into the influence of changes of ovarian hormones on the pathogenesis of the specific sub-type premenstrual syndrome(PMS)and reveal partial microcosmic mechanisms of adverse flow of liver-qi.Methods:Estradiol(E2)and progesterone(P)levels in serum were determined at different phases of menstrual cycle by radioimmunoassay.Results:In the group of PMS with adverse flow of liver-qi.the secretive peak value Of E2 and P at the follicular phase significantly decreased,and the secretive peak value at the luteal phase did not come into being.Conclusions:Low E2 and P secretive peak at the follicular phase and absence of secretive peak at the luteal phase is one of the microcosmic mechanisms of PMS with adverse flow of liver-qi.One of the pathophysiologic mechanisms of specific sub-type PMS is probably the continuous low level of E2and P. 相似文献
19.
Real-time three-dimensional echocardiography (RT3DE)is a new ultrasound technique that enables dynamic threedimensional visualization and quantification of the heart in real time. Investigation of feasibility and methodology of RT3DE in determining left ventricular (LV) and right ventricular (RV) volumes, RT3DE was performed in 35 normal adults using Philips SONOS 7500 system with a 2-4 MHz matrix array transducer. The 60°×60° "pyramid" volume database was obtained and analyzed on a TomTec echo workstation. Both LV and RV volumes were calculated with four 3DE methods (i.e. apical 2, 4, 8, and 16-plane) through manually tracing ventricular endocardial borders in end diastole and end systole. Stroke volumes were then calculated. LV volume was also measured by 2DE Simpson's rule using GE VIVID 7 ultrasound machine. 相似文献
20.
Increasing maternal age is the only etiological factor unequivocally linked to Down's syndrome in humans. The occurrence rate of newborns with Down's syndrome is about 1/220 in women over 35 years old. However, the occurrence rate in embryos fertilized in vitro, of the elder woman is unclear. Using FISH we screened the number of chromosome 21 in preimplanted embryos of 5 elderly women (average age, 38.4 years) to study the feasibility and necessity of screening trisomy 21 in embryos in patients over 35 years old at the in vitro fertilization (IVF) center. 相似文献