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1.
报道了一个同时测定转化胆甾醇发酵液中雄甾-4烯-3,17二酮(4AD)、雄甾-1,4二烯-3,17二酮(ADD)和胆甾醇的气相色谱内标法。使用FID检测器。玻璃柱长1.6m,内径3mm,内装涂有2%OV-17的60~80目Cromosorb W(AW-DMOS)担体。进样口温度285℃,柱温275℃。以氮作载气,流量50ml/min,用丙酸睾丸酮作内标物。在实验条件下,发酵液中各主要成分和杂质分离良好,便于定量。结果表明,4AD、ADD和胆甾醇的浓度与Ai/As的线性范围:4AD为0.1~1.8mg/ml(γ=0.9993);ADD为0.1~1.8mg/ml(γ=0.9994);胆甾醇为0.2-3.6mg/ml(γ=0.9991)。平均回收率依次为97.91±2.34(SD)%,95.88±1.21(SD)%,100.3±1.93(SD)%。变异系数分别为2.39%、1.26%、1.92%。  相似文献   

2.
样品溶液的制备及分析方法称取粉碎后样品500mg加50%甲醇40ml在水浴上回流提取1h,趁热过滤,滤液和洗液合并至50ml,取20ml通过填充了CM-(?)CH的柱(12mm×30mm),该柱用50%甲醇20ml清洗后,用0.1mol/LHCL洗脱并定容至20ml为样品溶液。内标溶液为L-肾上腺素的0.1mol/L HCI溶液(0.05mg/ml)。分析时取样品和标准溶液各1.0ml,加入内标溶液1.0ml,进样20μl。分析条件为:柱3011-C(弱酸性阳离子交换树脂4×250mm),流动相:0.1mol/L KH_2PO_4-0.3mol/L NH_4Cl-MeOH(35:35:30),流量1.0ml/min,检测220nm。在上述条件下,肾上  相似文献   

3.
目的 建立测定盐酸异丙嗪咖啡因片的含量及溶出度的高效液相色谱法.方法 色谱柱:Agilent TC C18柱(250 mm×4.6 mm,5μm);流动相:甲醇-三乙胺水溶液(浓度为3‰,磷酸调至pH2.3)=(50:50);流速:1.0 ml/min;检测波长分别为250和272 nm;柱温:30℃;进样量20μl(溶出度测定时进样量为10 μl).溶出条件采用桨法,温度为37℃,分别以900 ml pH1.2盐酸、pH 4.5醋酸缓冲液、pH 6.8磷酸缓冲液及水为溶出介质,以50、75 r/min作为转速进行溶出条件的筛选.结果 该HPLC检测方法专属性良好;盐酸异丙嗪、咖啡因分别在0.5 ~ 100 μg/ml和4.0 ~ 400 μg/ml范围内线性关系良好,线性回归方程分别为Y=96.21X-7.303(r=1)、Y=51.33X +68.88(r=0.9999);盐酸异丙嗪检测限为15 ng/ml,定量限为40 ng/ml;咖啡因检测限为2 ng/ml,定量限为10 ng/ml.平均回收率分别为盐酸异丙嗪(100.04±1.39)%(n=9),咖啡因(99.42±1.07)%(n=9);供试溶液在12h保持稳定.确立了以900 mlpH 1.2盐酸为溶出介质,桨法转速为50 r/min的溶出方法,溶出时间30 min.制剂在4种溶出介质中溶出度均在15 min内达85%以上,其溶出不受体液pH影响.结论 所选溶出条件适用于盐酸异丙嗪咖啡因片的溶出测定.所建含量及溶出度检测方法简便、快速、灵敏,精密度高,重现性好,结果准确,适合同时对盐酸异丙嗪及咖啡因进行含量及溶出度分析.  相似文献   

4.
[目的]建立炎琥宁原料药中的钠钾比测定方法.[方法]选取不同厂家的炎琥宁原料药,采用ICS-5000离子色谱系统,以IonPac AS 12A分析柱,IonPac AG12A为保护柱,甲烷磺酸(MSA)作为淋洗液,流速为1.0ml/min,样品稀释过滤后直接进样分析.[结果]钠、钾离子测定方法的加标回收率分别为96%和96.8%,线性相关系数为99.99%.[结论]本法简便、灵敏、准确,适用炎琥宁原料药中的钠钾比测定.  相似文献   

5.
目的 采用高效液相色谱(HPLC)外标法测定头孢氨苄干混悬剂中头孢氨苄的含量.方法 采用安捷伦1100色谱系统,色谱柱为C18 ODS柱(250×4.6 mm,5μm),流动相为水-甲醇-3.86%醋酸钠-4%醋酸(742:240:15:3),检测波长为254nm,进样量为15μ1,流速为1ml/min.结果 头孢氨苄...  相似文献   

6.
色谱条件为氢焰离子化检测器,不锈钢填冲柱2m×3mm,担体Cromosorb W AW DMCS 80~100目;固定液R-400 5%;气化室温度170℃,进样口170℃,层析柱100℃;流速为N_2 30 ml/min,H_2 35 ml/min,空气300ml/min。薄荷脑的回收率为97.8%,水杨酸甲酯为98.5%(n=3),CV<4%。五批样品的测定结果表明,薄荷脑及水杨酸甲酯含量差异较大,因其易挥发,对不同贮  相似文献   

7.
顶空气相色谱法测定二氯乙酸二异丙胺尿药浓度   总被引:2,自引:0,他引:2  
目的:建立顶空气相色谱法测定尿中二氯乙酸二异丙胺浓度.方法:Agilent DB-5MS毛细管色谱柱(30m×0.25mm),柱温:40℃保持2min,以5℃/min升至80℃保持2min,再以20℃/min升至200℃保持8min;进样口温度200℃,分流比5:1;氢火焰检测器,检测温度300℃;载气为高纯N2,流速1ml/min,H235ml/min,空气350ml/min;内标仲丁醇.结果:标准曲线线性范围为8~800μg/ml,尿中二氯乙酸二异丙胺提取回收率为88.75%~98.06%,相对回收率为97.36%~103.25%,日内和日间RSD分别为2.95%~6.62%和2.45%~5.61%,最低检测浓度为2μg/ml.结论:该法操作简单,杂质干扰小,提取回收率高,适合于二氯乙酸二异丙胺尿药浓度的测定.  相似文献   

8.
本文采用气相色谱法测定了麝香风湿油中两主成分的含量。测定条件为固定液:5%R 400;柱型:2m×3φ;柱温:122℃;鉴定器:氢火焰鉴定器;进样器温度:170℃;氮气:35ml/min;氢气:0.6ks/cm~2。本文测得薄荷脑的回收率为99.27%。变异系数为2.5%;水杨酸甲酯的回收率为98.59%.变异  相似文献   

9.
[目的]采用高效液相色谱法测定板蓝根颗粒中表告依春的含量.[方法]采用C18柱,色谱柱为Hypersil ODS2柱(250mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸水(10∶90),流速为1.0 ml/min,柱温为30℃,检测波长为245 nm,进样量10μl.[结果]表告依春的线性范围为10.0~60.0 μg/ml(A=341.58 C-429.9,r=0.9997),平均回收率为99.7%,RSD为0.42%.[结论]该方法简便,灵敏度高,稳定可靠,可以用于板蓝根颗粒中表告依春的质量控制.  相似文献   

10.
[目的]建立高效液相色谱法测定醋酸奥曲肽中奥曲肽含量的方法.[方法]色谱柱:ZORBAX 300SB-C8柱(2.1mm×150mm,5μm),流动相:A:0.1%TFA水B:0.1%TFA乙腈,流速:0.25 ml/min,柱温:40℃,检测波长:210nm,进样量:20μl.[结果]奥曲肽浓度在0.08 ~ 0.2 mg/ml范围内,线性关系良好,r=0.9999;检测限为0.02 mg/ml;加样回收率平均为101.28%,RSD为0.58%.[结论]分析方法可行,准确度高,此法可用于醋酸奥曲肽中奥曲肽含量的测定.  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.
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.
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.
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.
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   

18.
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   

19.
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   

20.
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   

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