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     

高效液相色谱法测定戊己丸中吴茱萸碱和吴茱萸次碱含量

目的　建立高效液相色谱法测定戊己丸中吴茱萸碱和吴茱萸次碱含量的方法。方法　采用高效液相色谱法。IntersilC18分析色谱柱 (4.6mmID× 2 5 0mm ,粒径 5 μm) ,流动相 :乙腈 - 10 %乙腈 (5 0 :5 0 ) ,流速 :1ml/min ,检测波长 :2 2 5nm。 结果　吴茱萸碱和吴茱萸次碱的理论板数分别为 2 6 81和 2 0 6 7。吴茱萸碱回归方程 :Y =0 .0 76 4 6 +0 .0 0 0 0 0 0 196 5X ,r=0 .9999) ,线性范围 10 .2～ 5 1.0 μg·ml-1;吴茱萸次碱回归方程 :Y =- 0 .2 199+0 .0 0 0 0 0 0 36 5 8X ,r =0 .9999) ,线性范围 10 .0～ 5 0 .0 μg·ml-1。吴茱萸碱平均回收率为 97.3% ,RSD 3.2 % ,吴茱萸次碱平均回收率为 10 1.4 % ,RSD 3.9%。吴茱萸碱和吴茱萸次碱最低检出浓度分别为 0 .0 5和 0 .1μg·ml-1。结论　方法简便 ,结果准确。     

反相离子对HPLC法测定晕宁贴膏中氢溴酸东莨菪碱的含量

目的　建立晕宁贴膏的含量测定方法。方法　采用ODSC18色谱柱 (2 5 0mm× 4 .6mm ,5 μm) ,以甲醇 -水 (含 0 .0 2 5mol·L-1庚烷磺酸钠及 0 .0 5mo1·L-1醋酸钠 ,以醋酸调pH =4 .6 ,) (4 5∶5 5 ) ,为流动相 ;流速 :1.0ml/min ;检测波长 :2 2 7nm ;柱温 :室温 ;外标法测定。结果　氢溴酸东莨菪碱在 1.32～ 13.2 μg范围内线性关系良好 (r =0 .9999) ;平均回收率 99.0 7% ,n =6 ,RSD为 0 .5 8% ;重现性试验RSD为 0 .5 0 %。结论　此方法简便、快速、准确 ,可作为晕宁贴膏的含量测定方法。     

高效液相色谱法测定解毒固本颗粒中大黄素和大黄酚含量

目的　建立高效液相色谱法测定解毒固本颗粒中大黄素和大黄酚含量的方法。方法　MZC18分析色谱柱 (4 .6mmID× 2 5 0mm ,粒径 5 μm) ,流动相A :10 %乙腈 (含 0 .5 %三乙胺 ,磷酸调pH3.0 ) ;B :85 %乙腈 (含 0 .5 %三乙胺 ,磷酸调pH3.0 )。梯度洗脱程序 :1～ 11min ,A :4 0 %～ 0 ;B :6 0 %～ 10 0 % ,流速 1.5ml/min。检测波长 4 33nm ;结果　大黄素回归方程Y =- 0 .0 0 14 75+0 .0 0 0 0 0 0 0 2 6 33X ,r =0 .9999,线性范围 0 .0 16 6 4～ 0 .6 6 5 4 μg ;大黄酚回归方程Y =- 0 .0 0 346 4 +0 .0 0 0 0 0 0 0 2 4 82X ,r =0 .9999,线性范围 0 .0 2 4 4 7～ 0 .9789μg。大黄素和大黄酚平均回收率分别为 96 .2 % (RSD =4 .7% )和 97.4 % (RSD =2 .1% )。结论　该方法操作简便 ,测定结果准确可靠 ,可用于测定解毒固本颗粒中大黄素和大黄酚含量。     

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     

HPLC法同时测定复方尼泊金乙酯醇溶液中二种组分的含量

目的　建立HPLC法同时测定复方尼泊金乙酯醇溶液中尼泊金乙酯及尼泊金甲酯含量的方法。方法　以ODSHypersil(5 μm ,2 0 0mm× 4 .6mm)为色谱柱 ,0 .0 1mol·L-1磷酸二氢钾 (KH2 PO4)溶液 -甲醇 -磷酸 (5 0∶5 0∶0 .4 )为流动相 ,检测波长 2 5 5nm。结果　一次进样即可完成两种组分的含量分析 ,线性范围 :尼泊金乙酯为 3.0 2 4～ 30 .2 4 μg·ml-1(r =0 .9999) ;尼泊金甲酯为1.0 2 2～ 10 .2 2 μg·ml-1(r=0 .9999)。平均回收率为 :尼泊金乙酯 99.4 5 % ,RSD =0 .4 8% (n =6 ) ;尼泊金甲酯 99.6 7% ,RSD=0 .72 % (n =6 )。结论　本方法快速、准确 ,分离度好。可用于该醇溶液中两种组份的含量测定。     

高效液相色谱法测定蛇花颗粒中绿原酸的含量

目的　建立蛇花颗粒中绿原酸的含量测定方法。方法　采用高效液相色谱法 ,以ZORBAXSB -C1 8(4 .6mm× 2 5 0mm ,5 μm)为色谱柱 ;流动相 :乙腈 - 0 .4 %磷酸溶液 (1 3∶87) ;检测波长 :32 7nm ;柱温 :2 5℃ ;结果　绿原酸在 0 .0 4 4 2～ 0 .4 4 2 0 μg范围内 ,浓度与峰面积线性关系良好 (r=0 .9998) ;样品的平均加样回收率为 :99.36 % ,RSD 为 1 .36 % ,(n=6 )。结论　方法简便、快速 ,可作为蛇花颗粒中绿原酸的含量测定方法     

反相高效液相色谱法测定复方汉防己颗粒中黄芪甲苷的含量

目的　建立反相高效液相色谱法测定复方汉防己颗粒中黄芪甲苷的含量。方法　采用AlltechC18(2 5 0mm× 4 .6mm ,5 μm)色谱柱 ,流动相 :乙腈 -水 (33∶6 7) ,流速 1ml/min ,柱温 :30℃ ,检测器 :ELSD2 0 0 0。 结果　黄芪甲苷在 0 .976～ 4 .88μg范围内线性关系良好 ,r=0 .9997,RSD =2 .1% ,回收率为 98.10 %。结论　本方法简便、灵敏准确、重现性好 ,可用于控制复方汉防己颗粒的质量。     

高效液相色谱法测定肝泰康胶囊中黄芩苷的含量

目的　测定肝泰康胶囊中黄芩苷的含量。方法　采用高效液相色谱法。色谱柱为DiamonsilC1 8柱 (2 5 0mm× 4 .6mm ,5 μm) ;甲醇 -水 -磷酸 (4 7∶5 3∶0 .1 )为流动相 ,流速 :1 .0ml/min ;检测波长 2 74nm。 结果　黄芩苷在 0 .1 2～ 1 .2 μg范围内具有良好线性关系 ,平均回收率为 97.4 7% ,RSD =1 .35 %。结论　该法可用于肝泰康胶囊中黄芩苷的含量测定     

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.     

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).     

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.     

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.     

Prevalence and severity of hip and groin pain in sub‐elite male football: a cross‐sectional cohort study of 695 players

The purpose of this study was twofold: (a) to investigate the prevalence of hip and groin pain in sub‐elite male adult football in Denmark and (b) to explore the association between prevalence and duration of hip and groin pain in the previous season with the Copenhagen Hip and Groin Outcome Score (HAGOS) in the beginning of the new season. In total 695 respondents from 40 teams (Division 1–4) were included. Players completed in the beginning of the new season (July–Sept 2011) a self‐reported paper questionnaire on hip and/or groin pain during the previous season and HAGOS. In total 49% (95% CI: 45–52%) reported hip and/or groin pain during the previous season. Of these, 31% (95% CI: 26–36%) reported pain for >6 weeks. Players with the longest duration of pain during the previous season had the lowest HAGOS scores, when assessed at the beginning of the new season, P < 0.001. This study documents that half of sub‐elite male adult football players report pain in the hip and/or groin during a football season. The football players with the longest duration of pain in previous season displayed the lowest HAGOS scores in the beginning of the new season.     

Bronchial stump fistula :treatment with covered retrievable hinged metallic stents-preliminary clinical experience

Objective To evaluate the preliminaily clinical efficacy and retrievability of a retrievable hinged covered metallic stent in the treatment of the bronchial stump fistula （BSF）. Methods Between April 2003 and March 2005, 8 patients with bronchial stump fistula after pneumonectomy or lobectomy were treated with two types （A and B） of retrievable hinged covered metallic stents. Type A stent was placed in 6 patients and type B in 2 under fluoroscopic guidance. The stent was removed with a retrieval set when BSF was healed or complications occurred. Results Stent placement in the bronchial tree was technically successful in all patients, without procedure-related complications. Immediate closure of the BSF was achieved in all patients after the procedure. Stents were removed from all patients but one. Removal of the stents was difficult in two patients due to tissue hyperplasia. Patients were followed up for 6 - 21 months. Placement of the stents remained stable in all patients except one due to severe cough. Permanent closure of BSF was achieved in 7 （87.5%） of 8 patients. Conclusion Use of a retrievable hinged covered expandable metallic stent is a simple, safe, and effective procedure for closure of the BSF. Retrieval of the stent seems to be feasible. （J Intervent Radiol, 2007, 16： 253-257）