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。     

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     

HPLC法测定湿疹净中霜公藤吉碱和苦参碱的含量

目的　建立湿疹净喷雾剂的质量控制标准。方法　采用HPLC法同时测定样品中雷公藤吉碱和苦参碱的含量。色谱条件 :HypersilODS色谱柱 (4.6× 2 5 0mm ,5 μm) ;流动相 :乙腈 - 0 .0 2mol·L-1磷酸二氢钠水溶液 (6∶4 ) ;流速 1ml/min ;检测波长2 10nm ;柱温 2 0℃ ;进样量 1～ 6 μl。结果　线性范围分别是 :雷公藤 0 .6 2 4～ 3.74 4 μg ,r =0 .9995 ;苦参碱 0 .88～ 5 .2 8μg,r =0 .9996。平均回收率 :雷公藤吉碱为 97.4 % ,RSD =1.5 1% ;苦参碱为 97.5 % ,RSD =1.15 %。结论　本方法测定结果准确、灵敏、重复性好     

胶束电动毛细管色谱法同时测定川芎中阿魏酸和腺苷的含量

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。     

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。     

HPLC法制备石杉碱甲

目的　建立用制备型HPLC制备石衫碱甲 (HuperzineA)的方法。方法　用常规的方法提取出石杉总生物碱。总生物碱经HPLC直接进样 ,柱子以 1 0 μSiO2 为填料 ,型号为 2 0× 30 0mm(Microsorb -MVTM) ,以氯仿 -甲醇 -氨水 (84 0∶2 4∶1 .2 )为流动相 ,流速为 8ml/min ,检测波长为 31 2 .7nm。结果　每次进样 3g石杉总生物碱 ,可以得到将近 1 80mgHuperzineA ,纯度达到 >90 %的工艺要求 ,重复性良好。结论　本方法与常规的分离方法比较 ,HPLC法制备石杉碱甲具有操作简单 ,重复性好 ,周期短 ,成本低廉等特点     

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     

肾康口服液的质量标准研究

目的　制订肾康口服液质量标准。方法　采用薄层色谱法 (TLC)等 ,对该制剂中黄柏、墨旱莲及总生物碱等进行定性鉴别 ;高效液相色谱法 ,对制剂中君药黄柏的有效成分盐酸小檗碱进行定量分析 ,选用NovapakC18柱 (2 .5cm× 4 .6mm ,5 μm) ,加NovapakC18预柱 (2 .5cm× 4 .6mm) ;流动相 :甲醇 -乙腈 - 0 .0 5mol·L-1磷酸二氢钠 (2 0∶35∶4 5 ) ;柱温 2 4℃ ;检测波长 346nm ;流速1.0ml/min。结果　采用TLC法鉴别 ,专属性强 ,含量测定盐酸小檗碱的线性范围为 4 .0 0～ 2 0 .0 0 μg·ml-1(r =0 .9992 ) ,平均回收率为 10 1.32 % ,RSD =1.18% (n =5 )。结论　本文方法简便 ,准确 ,重现性好。可有效地控制该制剂的质量     

高效毛细管电泳法同时测定苦豆子总碱注射液中3种生物碱的含量

目的应用高效毛细管电泳法测定苦豆子总碱注射液中苦参碱、氧化苦参碱、槐定碱的含量。方法运行缓冲液为100mmol·L-1硼砂,pH=9.2;运行电压8kV(恒压分析);柱温25℃;检测波长215nm;盐酸麻黄碱为内标。结果槐定碱、苦参碱、氧化苦参碱的线性范围分别为52.4～524、48.8～488、20.4～204μg·ml-1,平均回收率分别为98.22%、97.73%、98.82%,RSD分别为1.38%、2.15%、1.99%(n=6)。结论该方法简便、准确、重现性好,可作为苦豆子总碱注射液中生物碱的质量控制方法。     

二阶导数紫外分光光度法测定粉防己碱凝胶的含量

目的　建立粉防己碱外用凝胶制剂中粉防己碱的含量测定方法。方法　采用二阶导数紫外分光光度法 ,以 2 87nm波长处半振幅 (H)测定制剂中粉防己碱的含量。结果　粉防己碱在 10～ 5 0 μg·ml-1范围内 2 87波长处半振幅 (H)值呈良好线性关系 (r=0 .999) ,平均回收率 10 0 .0 5 % ,RSD 为 0 .132 %。结论　本法简单、准确、灵敏 ,能够排除凝胶辅料的干扰 ,可作为外用凝胶制剂质量控制方法     

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.