HPLC法测定黄柏石膏散中盐酸小檗碱含量

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     

洁康舒洗剂的质量标准研究

目的　制订洁康舒洗剂的质量标准。方法　采用薄层色谱法 (TLC)对该制剂中大黄、黄柏、徐长卿、冰片等主药进行定性鉴别 ,其中大黄的薄层鉴别以石油醚 -乙酸乙酯 -甲酸 (10∶3∶1)为展开剂 ;黄柏以正丁醇 -冰醋酸 -水 (10∶1∶1)为展开剂 ;徐长卿以环乙烷 -醋酸乙酯 (4∶2 )为展开剂 ;冰片以石油醚 -乙酸乙酯 (6∶2 )为展开剂。用高效液相色谱法测定该制剂中大黄酸、大黄素及大黄酚的含量 ,色谱柱为SymmetryC18柱 (3.9mm× 15 0mm ;5 μm) ,SymmetryC18预柱 (3.9mm× 2 0mm)流动相为甲醇 -水 -磷酸 (82∶18∶0 .1) ,柱温 2 4℃ ,检测波长 4 32nm ,流速为 1.0ml/min。结果　洁康舒洗剂中的有效成分与相应对照品均呈相同的鉴别反应 ,大黄酸、大黄素及大黄酚的浓度分别在 7.6 0～ 38.0 0 μg·ml-1(r =0 .9994 ) ;1.75～ 8.75 μg·ml-1(r =0 .9999) ;2 .4 0～ 12 .0 0 μg·ml-1(r =0 .9999)范围内线性关系良好。平均回收率大黄酸为 98.0 2 % ,RSD =1.78% ;大黄素为 96 .6 3% ,RSD =1.2 0 % ;大黄酚为 97.0 5 % ,RSD =1.15 % (n =5 )。结论　该制剂定性反应灵敏、TLC鉴别专属性强、定量结果准确、重现性好。本实验方法为洁康舒洗剂质量标准的制订提供了科学依据。     

高效液相色谱法测定胃必宁片中盐酸小檗碱和呋喃唑酮的含量

目的　建立测定胃必宁片中的盐酸小檗碱和呋喃唑酮含量的方法。方法　反相高效液相色谱法 :Nova -PakC18色谱柱 ,流动相为 0 .0 33mol·L-1磷酸二氢钾水溶液 -乙腈 (6 0∶4 0 ) ,检测波长为 2 6 5nm。结果　盐酸小檗碱和喃唑酮的含量在 4～2 5 μg·ml-1的浓度范围内线性关系良好 (r =0 .9999和r =0 .9998) ,样品的加样平均回收率分别为 99.2 8%和 99.0 8% ,RSD分别为 0 .6 7%和 0 .76 % (n =5 )。结论　所选方法简便、快速 ,可用于胃必宁片的质量控制     

高效液相色谱法测定烧伤Ⅱ号酊中盐酸小檗碱的含量

目的　建立反相高效液相色谱法测定烧伤Ⅱ号酊中盐酸小檗碱的含量。方法　固定相 :RP C18柱 ,流动相 :乙腈 醋酸乙酯 甲醇 0 .0 5mol·ml-1KH2 PO4溶液 (35∶10∶10∶6 5 ,加 1%三乙胺 ,磷酸调pH至 3.5 ) ,检测波长 :2 70nm。结果　盐酸小檗碱在0 .0 3～ 0 .10mg·ml-1浓度范围内 ,线性关系良好 ,r =0 .9996。日内及日间RSD分别为 1.5 5 %、2 .86 % (n =12 )和 1.78%、2 .6 5 % (n =4 ) ,加样回收率为 99.89% (RSD =1.18% )。结论　本法结果准确 ,灵敏度高 ,重现性好 ,可用于烧伤Ⅱ号酊剂中盐酸小檗碱的质量控制。     

高效液相色谱法测定心脉康注射液中人参皂苷Re的含量

目的　建立心脉康注射液中人参皂苷Re的含量测定方法 ,以控制其质量。方法　采用高效液相色谱法 ,HypersilC18柱 (15cm× 4 .6mm ,5 μm) ,以乙腈 - 0 .0 5 %磷酸溶液 (18∶82 )为流动相 ,检测波长 2 0 3nm。 结果　人参皂苷Re在 0 .0 5～ 1.2 5mg·ml-1范围内峰面积与其浓度呈良好线性关系 ,平均加样回收率为 99.6 % (RSD =1.8% )。结论　本法操作简便 ,准确可靠 ,可用于该制剂的质量控制。     

HPLC法同时测定菌克软膏盐酸林可霉素和硝酸咪康唑的含量

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。     

高效液相色谱法测定法莫替丁片溶出度

目的　测定法莫替丁片的溶出度。方法　高效液相色谱法 ,以Xterra -C18(3.9× 15 0mm ,5 μm)为色谱柱 ,流动相为庚烷磺酸钠溶液 -乙腈 -甲醇 (2 5∶6∶1) ,流速为 1.0ml/min ;检测波长为 2 5 4nm。结果　本品在 4 0～ 30 0 μg·ml-1范围内线性良好 (r=0 .9998) ,平均回收率为 99.6 5 % ,RSD =0 .4 %。结论　本法可排除辅料对溶出度测定的影响 ,可用于该制剂的质量控制。     

RP—HPLC法同时测定氯地滴眼液中氯霉素与地塞米松磷酸钠的含量

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。     

高效液相色谱法测定非那雄胺片的溶出度

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     

离子对-HPLC法测舒脉注射液中盐酸培他啶的含量

目的　建立离子对 -HPLC法测定舒脉注射液中盐酸培他啶含量的方法。方法　采用HypersilODS2色谱柱 (4 .6×2 5 0mm ,5 μm) ;以甲醇 - 1 0mmol·ml-1 醋酸钠溶液 (含有 5mmol·ml-1 庚烷磺酸钠 ,0 .2 %三乙胺 ,用冰醋酸调pH至 3.0 ) ,(4 0∶6 0 )为流动相 ;流速 1 .0ml/min ;检测波长 :2 6 0nm ;柱温为室温。结果　离子对 -HPLC法测定盐酸培他啶的线性范围为 2 1～ 1 0 5 μg·ml-1 ;相关系数 r=0 .9997;日内精密度 RSD =1 .5 % ,日间精密度 RSD =2 .6 % (n=5 ) ;平均回收率为 98.0 %。结论　本法简便、准确、专属性好     

Knee injury and Osteoarthritis Outcome Score (KOOS) - validation of a Swedish version

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.     

Endovascular management of carotid-cavernous fistulas

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.     

The acutely limping child

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.     

Do Balance Board Training Programs Reduce the Risk of Ankle Sprains in Athletes?

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).     

High Intensity Interval Training:New Insights

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).     

Developmental validation of the PowerPlex(®) ESI 16 and PowerPlex(®) ESI 17 Systems: STR multiplexes for the new European standard

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.