反相高效液相色谱法拆分醋酸棉酚对映异构体

目的建立醋酸棉酚的手性分析方法,用于拆分产物光学纯度的测定。方法采用高效液相色谱法,色谱柱为Chiralcel OD-RH手性柱(150 mm×4.6 mm,5μm),流动相为pH3.5磷酸三乙胺缓冲溶液-乙腈(体积比30∶70),流速为1.0 mL/min;检测波长为225 nm。结果醋酸棉酚消旋体在此条件下分离度为5.3。该方法用于手性拆分得到的光学对映体的光学纯度测定,对映体过量百分比(ee)在98%以上。结论本方法分离度、精密度和稳定性好,可用于一类抗肿瘤新药左旋(-)-醋酸棉酚原料药的合成反应监测、有关物质检测,及相关制剂的定量分析、有关物质检测,结果准确可靠。     

酮洛芬对映体的分离、分析方法的研究及其应用

目的:考察酮洛芬(Ketoprofen,KT)对映体在多糖衍生物手性固定相的色谱行为,建立酮洛芬对映体的分离分析方法,并用于血浆样品中酮洛芬对映异构体的测定.方法:色谱柱ChiralpakAD(250mm×4.6mm,10μm,Daicel Chemicals),流动相组成为正己烷:异丙醇:TFA(80:20:0.02),检测波长254 nm,流速1.0ml/min,柱温为25℃.结果:酮洛芬对映体在10min内实现分离,分离度大于2.0,对映体R和S分别在血药浓度0.1～10 μg/ml范围内线性关系良好R-(-)(r=0.9998),S-(+)(r=0.9996),单一对映体的最低检测限为2 ng(S/N=3).结论:建立了用ChiralpakAD柱分离分析酮洛芬对映异构体的方法,可用于单一对映异构体的光学纯度检测及药理学研究.     

罗通定与其右旋对映体的HPLC分离方法研究

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。     

纤维素手性固定相对联萘酚对映体的拆分

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,CHIRALPAKIC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:CHIRALPAKIC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。     

非索非那定对映体柱前手性衍生化反相高效液相色谱分析方法的建立

目的：建立适用于体外细胞模型的OATP1B1手性底物非索非那定柱前手性衍生化分析方法,为测定细胞中非索非那定对映体提供分析手段。方法：选择R-(+)-苯乙基异氰酸酯作为手性衍生化试剂,与非索非那定生成氨基甲酸酯衍生物,应用液相色谱-串联质谱法确定对映体衍生物色谱峰,通过反相高效液相色谱法实现对映体的分离分析。结果：在建立的手性分离条件下,成功实现非索非那定对映体分离分析,非索非那定两个对映体衍生物在25 ~100 ng/ml浓度范围内线性关系良好 (R²=0.9992, 0.9989),日内、日间精密度均小于10%。结论：本实验建立的非索非那定对映体柱前手性衍生化反相高效液相色谱分析方法灵敏、准确,可用于体外细胞模型中盐酸非索非那定立体选择性分析。     

克伦特罗和马布特罗在替考拉宁手性柱上的对映体分离

目的研究自制的替考拉宁手性色谱柱上对克伦特罗和马布特罗进行对映体分离,探讨其手性识别机理.方法在流动相组成的甲醇/乙醇/冰醋酸/三乙胺=50/50/0.05/0.05(V/V/V/V),流速1.0 mL/min,柱温25℃.应用了极性流动相中不同浓度的酸碱添加剂,不同浓度的乙醇,柱温和流速对克伦特罗和马布特罗对映体进行分离.结果在上述条件下,克伦特罗对映体和马布特罗对映体的选择因子分别达到1.37和1.51.结论自制的替考拉宁手性柱对克伦特罗和马布特罗的对映体具有一定的分离效果.     

体外细胞模型中氟伐他汀对映体的手性分离和含量测定方法学研究

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。     

羟丙基β环糊精毛细管电泳法测定1,2-二苯基乙二醇的对映体过量值

目的:建立毛细管电泳法(CE)测定(E)-1,2-二苯乙烯不对称二羟化反应产物1,2-二苯基乙二醇对映体过量(e.e.%)值的新方法.方法:以HP-β-CD为手性选择剂,采用毛细管区带电泳法研究背景电解质浓度、pH值、环糊精浓度、分离电压、温度等参数对1,2-二苯基乙二醇对映体分离的影响,同时对该合成样品进行光学纯度检查,并与HPLC测定结果作比较.结果:在200 mmol/L硼酸缓冲液(pH=9.8),15 mmol/L HP-β-CD,15 kV分离电压、柱温20℃的基本优化条件下,1,2-二苯基乙二醇对映体得到基线分离,Rs达到3.35.同时,该合成样品分析结果表明,4批样品的e.e.%测定值与HPLC法结果相一致.结论:该CE方法简单、准确,可用于该1,2-二苯基乙二醇的手性拆分和e.e.%值的测定.     

沙丁胺醇在3,4-二氯苯基异氰酸酯万古霉素手性柱上的对映体分离

目的建立一种在自制手性柱上对沙丁胺醇进行了对映体分离的方法.方法利用极性流动相中不同浓度的酸、碱添加剂在自制的3,4-二氯苯基异氰酸酯万古霉素手性柱对沙丁胺醇对映体分离的研究,初步探讨了手性识别机理.结果流动相中酸、碱添加剂的比例为0.01%:0.01%(V/V),流速为1 mL/min,柱温为25℃时,沙丁胺醇获得了最好的对映体分离,选择因子为1.16,分离度达到1.41.结论自制的3,4-二氯苯基异氰酸酯万古霉素手性柱对沙丁胺醇有一定的分离效果,可以此为参考,开发其他类似的手性固定相.     

毛细管电泳法检测美普他酚手性拆分中的光学纯度

目的 建立测定二对甲苯甲酰酒石酸美普他酚对映体的毛细管区带电泳法,并检测其光学纯度。方法 采用72 cm×50 μm未涂层石英毛细管,30 mmol／L磷酸缓冲液(pH 8.05,内含0.5％TM-β-CD,乙腈12％),运 行电压20 kV,毛细管柱温20℃,压力进样3 kPa×3 s,检测波长200 nm。结果 在选定的实验条件下二对甲苯 甲酰酒石酸美普他酚对映体达到基线分离。两对映体在0.10-0.80 mg/mL的浓度范围内,浓度与峰面积的响 应均呈良好的线性关系,相关系数分别为:0.999 6和0.999 8。迁移时间的RSD在3％以内,峰面积的RSD在 10％以内,左旋体的加样回收率为100.26％(n=6),最低检测浓度为0.02 mg／mL。测定3批样品的光学纯度 分别为84.10％、92.54％、≥99.60％。结论 本法适用于实验室中二对甲苯甲酰酒石酸美普他酚光学纯度的常 规测定。     

Value of D-Dimers in patients with acute aortic dissection

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.     

Research of combined liver-kidney transplantation model in rats

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.     

Development on Adjustable Calibration Marker for Shock Wave Focus

Shock wave lithotripsy （SWL） is a treatment of choice for upper urinary stones. However, this procedure is inappropriate for obese patients because the focus is often unable to reach the target owing to the limited focal distance in shock wave source. Although treating such patients in a blast path may increase the application length of shock wave source, it＇s difficult to find this path on the lithotripter monitor. For this reason, we invented an adjustable calibration marker in order to set an effective focus in the shock wave hath.     

Study on the TCM Pathogenesis of Angiopathic Complications of Type II Diabetes

Excess production of reactive oxygen species(ROS)of mitochondrion mediated by hyperglycemia is the common pathogenesis of angiopathic complications of diabetes.TCM holds that the damp from the dysfunction of spleen.kidney and liver is the causative factor of complications of diabetes.This is similar to the mechanism of Ros resulting in angiopathic complications of diabetes.When the angiopathic complications of type II diabetes mellitus(T2DM)are difierentiated as caused by turbid damp in TCM can be explained as ROS.Since the obstruction of pathogenic damp in channels and collaterals is said to be the main pathogenesis,the treating principle should be dissolving the damp to remove the obstruction.     

Leptin, Ghrelin and TNF-α before and after Hypo-caloric Traditional Chinese Diet and Auricular Acupuncture

INTRODUCTION Obesity is a complex emergent problem, which can be possibly solved not only by the diet but also by the life style and promotion of a constant physical exercise. 1, 2 No doubt careful attentions must be given to the nutritional condition of obese people, the dietary habits, the somatic build (i.e. distribution of fat mass) and the organic functions linked to formation of the fat mass. All the parameters should be constantly monitored before, during and after a diet treatment. 3, 4, 5     

Relationship between Dysglycemia and Carotid Atherosclerosis in Tibetan Population

People with dysglycemia are at high risk for atherosclerotic diseases. This study aims at investigating the atherosclerotic vascular damage in dysglycemia and its metabolic origin in Tibetan population.     

APPLICATION OF LORNOXICAM TO PATIENT-CONTROLLED ANALGESIA IN PATIENTS UNDERGOING ABDOMINAL SURGERIES

FOR anesthesiologis s ,treatingpostoperativepainhas alwaysbeen a problem.Althoughopioidshave been provedtobe effective,theirsideeffectscouldnotbeignored.With thedevelopmentofscienceand pharmacology,many drugs with aspectsof satisfactoryanalgesicefficacyand couldbe welltoleratedby patientshave been developed.And lornoxicamisone of them, which isa non-steroidalanti-inflammatorydrug (NSAID ), with analgesic, anti-infl-ammatory,andantipyreticproperties.Itseliminationhalf-time(3 to 5 hours) isle…     

安心颗粒对急诊经皮冠状动脉介入术后生活质量影响的研究

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.     

CLINICAL SIGNIFICANCE OF SERUM CYTOKINES IL-1β,sIL-2R,IL-6,TNF-α,AND IFN-v IN ACUTE CORONARY SYNDROME

Objectives To explore serum cytokines levels (including IL-1 β, sIL-2R, IL-6, TNF-α, and IFN-v) and their significance in patients with acute coronary syndrome (ACS) and the subsequent follow-ups, with attempt to estimate the role of various serum inflammatory markers in the diagnosis and assessment of ACS.Methods The study population include 40 patients with acute myocardial infarction (AMI), 40 patients with unstable angina pectoris (UAP), and 40 controls. Among the 80 patients, 60 patients attended a follow up 4 months later. Serum inflammatory markers including IL-1 β, sIL-2R, IL-6, TNF-α, and IFN-v were measured by enzyme linked immunosorbent assay.Results Serum IL- 1 β, sIL-2R, IL-6, TNF-α were significantly higher in AMI group or UAP group compared to the control group and became significantly lower 4 months later in the follow-up patients. Serum levels of IFN-v shows no significant difference between AMI group or UAP group and controls, also showing no significant change when measured in follow up patients. There was no correlation between serum creatine kinase-MB isoenzyme levels and serum inflammatory markers either in UAP or AMI group. Furthermore, when divided into two subgroups using Wagner's QRS scoring system in the AMI group, there is no difference of each serum inflammatory marker between ≤ 6 scores group and ＞ 6 scores group.Conclusion Serum levels of certain inflammatory markers may have some diagnostic value for ACS, and can be a useful marker reflecting disease stability.     

Possible Spread of adenovirus type 3 from poultry to humans ：indirect evidence from an outbreak in China

Objective:To explore the epidemiology and etiology for an outbreak of acute respiratory tract infection that occurred in one county of Jiangsu Province, China 2004. Methods: Only cases meeting the case definition were included in the study. We reviewed the medical records of the cases who were admitted to the local hospitals, interviewed cases by a standard questionnaire, and then described the epidemiotogic features and analyzed risk factors by means of a case-control study. We collected pharyngeal swab specimens and sent them to different laboratories for isolation and culture. The laboratory used different detection methods such as DIP, PCR, electron microscope examination and microneutralization assay, to identify and then type the positive specimens. Results:A total of 871 cases were reported during the period from April 18 to July 4,2004. The distribution of onset times presented two peaks, one in late May and another in middle June. The epidemic occurred mainly in the elementary and junior high schools in ten townships of one county, and the mean age of the cases was 12 years (range 7 months to 18 years). The course of the disease was acute, and was characterized by fever accompanied with sore throat and tonsillitis. The WBC count of cases was normal or elevated. The mean duration of illness was 5 days (range 2 to 12 days). No fatalities from illness were reported. A case-control study indicated that the possible risk factors were close contact with a case and/or poultry before onset and sharing of towels among members of the family. The typical CPE was observed through inoculating pharyngeal swab specimens into the HEP-2 cell cultures in different laboratories. An infection of adenovirus type 3 was verified by detecting positive specimens in different methods. Conclusion:This investigation demonstrated that the acute respiratory infection in cases was caused by adenovirus type 3. Cases occurred in over 70 schools in ten townships in 2004, and the route of transmission was possibly close contact with cases or droplet transmission.