重组人干扰素α-2b两步柱色谱分离纯化工艺研究

通过改进柱色谱条件,两步柱色谱分离纯化重组人干扰素α-2b,简化了工艺,缩短了生产流程,纯化倍率达到5.6倍,纯度98%.蛋白比活性1.43×108IU/mg蛋白,活性回收率58%.     

那格列奈及其片剂中L-异构体的HPLC测定

建立了HPLC法测定那格列奈及其片剂中的杂质L-异构体的含量.采用以α-酸性糖蛋白键合硅胶为固定相的手性色谱柱,0.02mol/L磷酸钾缓冲液(pH 7.1)-乙腈(98:2)为流动相,检测波长210nm,L-异构体检测限为2ng,平均回收率为98.0%.     

髋臼双柱骨折合并后壁骨折的手术治疗

目的 探讨髋臼双柱合并后壁骨折的临床特点和手术疗效.方法 对29例髋臼双柱合并后壁骨折采用双切口分步入路切开复位,重建钢板内固定.结果 按Matta标准,解剖复位21例,满意复位5例,不满意复位3例.随访13～38个月,平均19个月,关节功能按d'Aubinge-Possel评分系统评定,优17例,良6例,可3例,差3例.结论 双切口分步入路,重建钢板固定是治疗髋臼双柱合并后壁骨折的有效方法.     

脊柱放线菌感染并发脊髓压迫症(附3例报告)

目的探讨脊柱放线菌感染并发脊髓压迫症的临床和影像学特点及治疗方法。方法回顾性分析3例经病理检查证实的本病患者的临床资料。结果3例患者均有颈、胸脊椎及软组织感染和脊髓压迫症状;MRI示病变椎体骨质破坏,颈、胸硬膜外软组织肿块,脊髓受压。病理学检查组织病理学检查证实3例均为放线菌感染,2例表现为炎性肉芽组织伴微脓肿形成,另1例表现为硬膜外脓肿。均予以脓肿清除、脊髓减压术,并给予4~8周大剂量青霉素G静脉滴注,后改口服维持4~6个月,术后及随访3例患者均取得显著的疗效。结论脊柱放线菌感染并发脊髓压迫症临床和影像学表现无特征性,其确诊依赖于病理学和微生物学检查。脓肿引流、椎管内减压术和大剂量抗生素治疗有效。     

免疫亲和柱净化HPLC柱后光化学衍生法测定34批中药材中黄曲霉毒素G_2、G_1、B_2、B_1

目的建立HPLC柱后光化学衍生法检测中药材中黄曲霉毒素G2、G1、B2、B1方法。方法样品经过70%甲醇提取、免疫亲和柱净化后,采用HPLC柱后光化学衍生-荧光检测器检测中药材黄曲霉毒素含量。对疑似成分进行液质确认。结果黄曲霉毒素G2和B2,G1和B1分别在0.75～22.5 pg和5～75pg线性关系良好,方法准确稳定。检测的34批次药材中,3批酸枣仁检出黄曲霉毒素,其中1批酸枣仁黄曲霉毒素B1超过5μg·kg-1。结论该方法简便、准确,适用于中药材黄曲霉毒素的检测。     

超临界流体色谱法测定碘帕醇的对映异构体

目的 用超临界流体色谱法(SFC)测定碘帕醇的对映异构体。方法 采用Chiralpak OD-H手性色谱柱,以CO2：甲醇(89∶11)为流动相,检测波长为242 nm。结果 R-碘帕醇在0.2~1.2 mg/ml范围内线性关系良好,精密度及回收率良好(精密度RSD=1.2%,n=6;回收率103.7%,RSD=0.7%,n=9)。且R-碘帕醇与S-碘帕醇分离度良好。结论 本法快速、准确、可靠、专属性强,可用于碘帕醇中R-碘帕醇的控制。     

盐酸芬氟拉明对映体的柱前衍生物GC法分析

以ω－莰烷酰氯为衍生试剂,采用柱前衍生化ＧＣ法,成功地分析了盐酸芬氟拉明、金刚乙胺和盐酸氯胺酮。光谱分析确证了芬氟拉明酰胺衍生物的结构,优化了盐酸芬氟拉明酰胺衍生物的结构,优化了盐酸芬氟拉明衍生条件,建立了盐酸花氟拉明的内标法定量分析方法。     

Vertical split fracture of the vertebral body following oblique lumbar interbody fusion: A case report

Rationale:Oblique lumbar interbody fusion (OLIF) is an effective and safe surgical technique widely used for treating spondylolisthesis; however, its use is controversial because of several associated complications, including endplate injury. We report a rare vertebral body fracture following OLIF in a patient with poor bone quality.Patient concerns:A 72-year-old male patient visited our clinic for 2 years with lower back pain, leg radiating pain, and intermittent neurogenic claudication.Diagnoses:Lumbar magnetic resonance imaging revealed L4-5 stenosis.Intervention:We performed OLIF with percutaneous pedicle screw fixation and L4 subtotal decompressive laminectomy. We resected the anterior longitudinal ligament partially for anterior column release and inserted a huge cage to maximize segmental lordosis. No complications during and after the operation were observed. Further, the radiating pain and back pain improved, and the patient was discharged. Two weeks after the operation, the patient visited the outpatient department complaining of sudden recurred pain, which occurred while going to the bathroom. Radiography and computed tomography revealed a split fracture of the L5 body and an anterior cage displacement. In revision of OLIF, we removed the dislocated cage and filled the bone cement between the anterior longitudinal ligament and empty disc space. Further, we performed posterior lumbar interbody fusion L4-5, and the screw was extended to S1.Outcomes:After the second surgery, back pain and radiating pain in the left leg improved, and he was discharged without complications.Lesson:In this case, owing to insufficient intervertebral space during L4-5 OLIF, a huge cage was used to achieve sufficient segmental lordosis after anterior column release, but a vertebral body coronal fracture occurred. In patients with poor bone quality and less flexibility, a huge cage and over-distraction could cause a vertebral fracture; hence, selecting an appropriate cage or considering a posterior approach is recommended.     

哈士蟆卵油化学成分研究

哈士蟆油 (ｏｖｉｄｕｃｔｕｓｒａｎａｅ)为中国林蛙(ＲａｎａｔｅｍｐｏｒａｒｉａｃｈｅｎｓｉｎｅｎｓｉｓＤａｖｉｄ .)雌蛙的干燥输卵管制品 ,系一种名贵中药材 ,对它的化学成分和药效作用研究已有综述报道[1 ] 。但中国林蛙卵 ,民间用其治疗肺虚咳嗽 ,其化学成分至今未见报道。为开发利用这一资源 ,本文以林蛙卵为原料 ,对其脂溶性部分的化学成分进行了初步研究。化合物Ｒｌ 1 :白色针状结晶 (石油醚 乙酸乙酯 ) ,ｍｐ 1 48～ 1 5 0℃ ,Ｌｉｅｂｅｒｍａｎｎ Ｂｕｒｃｈａｒｄ反应阳性。1 Ｈ ＮＭＲ (ＣＤＣｌ3)δ :0 68(ｓ,3Ｈ ,Ｃ…     

栀子提取物中大孔吸附树脂的苯残留量检查

目的测定栀子提取物中大孔吸附树脂残留的苯是否符合限量要求.方法使用气相色谱仪,采用DB-624毛细管色谱柱,以氮气为载气,FID检测器,测定苯.结果栀子提取物中未检出苯,检出限为0.06mg·L-1.结论该方法简便、准确、重复性好,可用于栀子提取物的质量控制.