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1.
毛细管电泳法测定当归及其制剂中阿魏酸的含量   总被引:5,自引:0,他引:5  
目的 建立HPCE法测定当归及其制剂中阿魏酸含量的方法。方法 空心熔融石英毛细管 (75 μm× 1 0 0cm) ,1 0mmol·L-1 硼砂溶液为电泳介质 ,30kV运行电压 ,温度 2 5℃ ,重力进样 5s,检测波长 2 1 4nm。结果 阿魏酸在 5~ 1 0 0 μg·ml-1 范围内 ,可定量检测。回归方程为 :Y =- 7.735 +0 .0 2 6 3X ,r=0 .9993,精密度试验 RSD 为 2 .5 9% ,样品重复性 RSD 为 1 .2 0 % ,三种样品含量的RSD为 2 .2 9%。结论 毛细管电泳法可用于当归及其制剂中阿魏酸的测定 ,方法简便 ,可行  相似文献   

2.
目的 利用反相离子对液相色谱法测定复方降压胶囊中磷酸氯喹的含量。方法 采用HYPERSILODS2 (4 .6× 2 5 0mm ,5 μm)色谱柱 ,乙腈 -甲醇 -己烷磺酸钠溶液 (18∶18∶6 4 )为流动相 ,流速为 1.0ml/min ,检测波长 343nm。 结果 磷酸氯喹线性范围为 :2 1.6~ 2 81μg·ml-1,r=0 .9999;日内精密度 RSD 为 0 .4 2 % (n=6 ) ;日间精密度 RSD 为 0 .5 5 % (n=5 )。平均回收率为97.1% (n =9)。结论 本方法简便 ,准确 ,适用于该药的质量控制  相似文献   

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目的 建立RP -HPLC法测定尼莫地平片的含量及含量均匀度。方法 色谱柱ODS -C18柱 ,流动相为甲醇 -水 (80∶2 0 ) ,检测波长为 2 38nm。结果 在 2 .5~ 32 μg·ml-1浓度范围内呈良好的线性关系 ,平均回收率为 99.6 3% ,RSD为 0 .98%。结论 该法专属性强 ,操作简便 ,结果准确  相似文献   

4.
目的 建立高效液相色谱法同时测定菌克软膏中盐酸林可霉素和硝酸咪康唑的含量。方法 采用高效液相色谱法 ,HYPERSIL -CN色谱柱 (5 μm ,4 .6mm× 2 0 0mm) ,流动相 0 .0 5mol·L-1硼砂溶液 (用磷酸调节pH至 6 .0 ) -甲醇 (85∶15 ) ,流速 1.0ml/min ;检测波长 2 14nm ;进样量 10 μl。 结果 盐酸林可霉素在 0 .0 8~ 3.2mg·ml-1浓度范围内均呈良好的线性关系 ,r =0 .9999(n =5 ) ,硝酸咪康唑在 0 .0 8~ 1.6mg·ml-1范围内呈良好的线性关系 ,r =0 .9993(n =5 )。盐酸林可霉素的平均回收率为 10 1.2 3% ,RSD为 0 .93% ,硝酸咪康唑的平均回收率为 99.82 % ,RSD为 0 .5 7%。结论 本方法分离度好 ,简便 ,准确 ,适用于软膏制剂中 2组分的同时测定 ,可作为产品的质量控制方法。  相似文献   

5.
目的 测定苯麻滴鼻液中盐酸苯海拉明及盐酸麻黄碱的含量。方法 采用旋光法测定盐酸麻黄碱 ,一阶导数光谱法测定盐酸苯海拉明。后者测试条件 :波长范围 2 0 0~ 30 0nm ,狭缝 2nm ,△λ =1nm ,振幅范围 - 0 .5~ +0 .5。结果 盐酸麻黄碱平均回收率 10 0 .15 % ,RSD =0 .38% (n =3) ;盐酸苯海拉明在 5~ 75 μg·ml-1范围内 ,浓度与一阶导数在 2 2 8nm波长处的半振幅值 (D)呈良好的线性关系 ,其回归方程为C =347.4 6 95D - 1.196 7,r =0 .9999,平均回收率 99.6 4 % ,RSD =0 .4 2 % (n =5 )。结论 本法准确、简便 ,可用于苯麻滴鼻液的质量控制  相似文献   

6.
HPLC法测定黄柏石膏散中盐酸小檗碱含量   总被引:3,自引:0,他引:3  
目的 建立测定黄柏石膏散中盐酸小檗碱含量的高效液相色谱法。方法 色谱柱 :IntersilC18柱 (4 .6mmID× 2 5 0mm ,5 μm) ;流动相 :水 -乙腈 (6 9∶31) ,用 0 .5 %三乙胺、磷酸调pH至 3.0 ;检测波长 35 0nm ;流速 :1ml/min。 结果 盐酸小檗碱的理论板数为 5 6 0 0。回归方程Y =- 2 .4 2 5 +0 .0 0 0 0 0 114 2X ,r =0 .9998。线性范围 5 1.2 0~ 2 5 6 .0 μg·ml-1。平均回收率为 10 1.4 % (n =5 ) ,RSD为 1.2 %。结论 该法操作简便 ,结果准确 ,可用于黄柏石膏散中盐酸小檗碱含量测定  相似文献   

7.
HPLC法测定盐酸纳洛酮鼻腔喷雾剂的含量及有关物质   总被引:3,自引:0,他引:3  
目的 建立HPLC法用于盐酸纳洛酮鼻腔喷雾剂的含量及有关物质测定。方法 色谱柱为ApolloODS (15 0× 4 .6 0mm ,5 μm) ;流动相为甲醇 -乙腈 - 0 .0 2mol·L-1的磷酸二氢钾 (1∶1∶8) ;流速 1.0ml/min ;检测波长 2 4 0nm ;外标法峰面积定量。结果 在该色谱条件下 ,中间体、辅料、分解产物等对主药测定无干扰 ;盐酸纳洛酮浓度在 10 .2~ 81.6 μg·ml-1范围内线性关系良好 ,回归方程为Y =110 2 6 .4 1X - 1982 3.96 ,r =0 .9998;最低检出浓度为 5 0ng·ml-1;高、中、低三个浓度日内、日间的RSD在0 .4 9%~ 1.5 1%之间 ;重复性试验RSD为 0 .98% (n =9) ;样品的平均回收率为 99.92 % ,RSD为 0 .70 % (n =9)。结论 该法准确、可靠、重现性好 ,可用于盐酸纳洛酮鼻腔喷雾剂的含量及有关物质的测定  相似文献   

8.
目的 采用高效液相色谱法测定非那雄胺片的溶出度。方法 高效液相色谱法。色谱柱为LUNA 5 μmC18(2 ) (15 0×4 .6 0mm ,U .S .A) ,流动相为 2 .5mmol·L-1磷酸溶液 -乙腈 (1∶1) ,检测波长 2 2 0nm。结果 非那雄胺的最低检出量约为 2ng ;非那雄胺在 1.4~ 16 .8μg·ml-1(r =0 .9999)范围内 ,峰面积与其浓度呈良好线性关系 ,平均回收率为 99.6 1% ,RSD为 1.0 5 % (n=6 )。结论 分析速度快 ,简单 ,结果准确可靠  相似文献   

9.
目的 建立胶束电动毛细管色谱法测定阿魏酸和腺苷含量。方法 用未涂层石英毛细管 5 0 μmi.d .× 5 6cm ,长度 4 7.5cm ;6 5mmol·L-1硼砂和 8mmol·L-1去氧胆酸钠 (pH9.5 ) ,并含有 5 %甲醇的缓冲液为电泳介质 ;操作电压 2 8kV ;毛细管柱温2 2℃ ;检测波长 :2 10nm。结果 阿魏酸和腺苷分别在 2 0~ 32 0、10~ 16 0 μg·ml-1浓度范围内线性关系良好 (r>0 .999) ;平均回收率分别为 99.0 %和 10 1% ;RSD在 6 %以内 (n =5 )。结论 胶束电动毛细管色谱法可用于川芎中阿魏酸和腺苷的含量测定。  相似文献   

10.
目的 建立测定氯地滴眼液中氯霉素和地塞米松磷酸钠含量的反相高效液相色谱法。方法 在Hypersil(2 5 0mm× 4 .6mm ,5 μm)色谱柱上 ,以甲醇 - 0 .0 5mol·L-1醋酸钠缓冲液 (pH =4 .0 ) (40∶6 0 )为流动相 ,紫外检测波长 2 4 0nm ,外标法定量。结果 同时测定 2组分的含量 ;氯霉素 0 .5~ 2 .0mg·ml-1,地塞米松磷酸钠 0 .1~ 0 .3mg·ml-1范围内 ,浓度与峰面积成良好的线性关系 ;平均回收率分别为 98.3% (RSD =0 .9% ) ,97.8% (RSD =0 .7% )。结论 本法操作简便 ,结果准确。  相似文献   

11.
The Knee injury and Osteoarthritis Outcome Score (KOOS) is a self-administered instrument measuring outcome after knee injury at impairment, disability, and handicap level in five subscales. Reliability, validity, and responsiveness of a Swedish version was assessed in 142 patients who underwent arthroscopy because of injury to the menisci, anterior cruciate ligament, or cartilage of the knee. The clinimetric properties were found to be good and comparable to the American version of the KOOS. Comparison to the Short Form-36 and the Lysholm knee scoring scale revealed expected correlations and construct validity. Item by item, symptoms and functional limitations were compared between diagnostic groups. High responsiveness was found three months after arthroscopic partial meniscectomy for all subscales but Activities of Daily Living.  相似文献   

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Objective To investigate endovascular treatment of traumatic direct carotid-cavernous fistulas (CCF) and their complications such as pseudoaneurysms. Methods: Over a five-year period, 22 patients with traumatic direct CCFs were treated endovascularly in our institution. Thirteen patients were treated once with the result of CCF occluded, 8 twice and 1 three times. Treatment modalities included balloon occlusion of the CCF, sacrifice of the ipsilateral internal carotid artery with detachable balloon, coll embolization of the cavernous sinus and secondary pseudoaneurysms, and covered-stem management of the pseudoaneurysms. Results All the direct CCFs were successfully managed endovascularly. Four patients developed a pseudoaneurysm after the occlusion of the CCF with an incidence of pseudoaneurysm formation of 18.2% (4/22). A total number of 8 patients experienced permanent occlusion of the ICA with a rate of ICA occlusion reaching 36.4% (8/22). Followed up through telephone consultation from 6 months to 5 years, all did well with no recurrence of CCF symptoms and signs. Conclusion Traumatic direct CCFs can be successfully managed with endovascular means. The pseudoaneurysms secondary to the occlusion of the CCFs can be occluded with stent-assisted coiling and implantation of covered stents.  相似文献   

15.
Acute limping may be the result of multiple pathologies in children. The differential diagnosis varies based on the age of the child. Irrespective of age, the initial imaging work-up includes AP and frog leg radiographs of the pelvis and ultrasound; MRI may sometimes be helpful. In children less than 3 years, infections and trauma are most frequent. MRI is the imaging modality of choice when osteomyelitis is clinically suspected. Between the ages of 3 and 10 years, transient synovitis of the hip and Legg-Calvé-Perthes disease are main considerations but infection, inflammation and focal bony lesions are also considered. In children over 10 years, slipped capital femoral epiphysis also is considered.  相似文献   

16.
Introduction Ankle sprains are the most common musculo-skeletal injury that occurs in athletes,particularly in sports that require jumping and landing on one foot such as soccer,and basketball(1-4).These injuries often result in significant time loss from participation,long-term disability,and have a major impact on health care costs and resources(5-8).  相似文献   

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KEY POINTS ·High-intensity interval training(HIT)is characterized by repeated sessions of relatively brief,intermittent exercise.often performed with an“a11 out”effort or at an intensity close to that which elicits peak oxygen uptake(i.e.,≥90%of VO2 peak).  相似文献   

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In response to the ENFSI and EDNAP groups’ call for new STR multiplexes for Europe, Promega® developed a suite of four new DNA profiling kits. This paper describes the developmental validation study performed on the PowerPlex® ESI 16 (European Standard Investigator 16) and the PowerPlex® ESI 17 Systems. The PowerPlex® ESI 16 System combines the 11 loci compatible with the UK National DNA Database®, contained within the AmpFlSTR® SGM Plus® PCR Amplification Kit, with five additional loci: D2S441, D10S1248, D22S1045, D1S1656 and D12S391. The multiplex was designed to reduce the amplicon size of the loci found in the AmpFlSTR® SGM Plus® kit. This design facilitates increased robustness and amplification success for the loci used in the national DNA databases created in many countries, when analyzing degraded DNA samples. The PowerPlex® ESI 17 System amplifies the same loci as the PowerPlex® ESI 16 System, but with the addition of a primer pair for the SE33 locus. Tests were designed to address the developmental validation guidelines issued by the Scientific Working Group on DNA Analysis Methods (SWGDAM), and those of the DNA Advisory Board (DAB). Samples processed include DNA mixtures, PCR reactions spiked with inhibitors, a sensitivity series, and 306 United Kingdom donor samples to determine concordance with data generated with the AmpFlSTR® SGM Plus® kit. Allele frequencies from 242 white Caucasian samples collected in the United Kingdom are also presented. The PowerPlex® ESI 16 and ESI 17 Systems are robust and sensitive tools, suitable for the analysis of forensic DNA samples. Full profiles were routinely observed with 62.5 pg of a fully heterozygous single source DNA template. This high level of sensitivity was found to impact on mixture analyses, where 54–86% of unique minor contributor alleles were routinely observed in a 1:19 mixture ratio. Improved sensitivity combined with the robustness afforded by smaller amplicons has substantially improved the quantity of data obtained from degraded samples, and the improved chemistry confers exceptional tolerance to high levels of laboratory prepared inhibitors.  相似文献   

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