复方丹参片显微定量及异性有机物检查方法改进的研究

目的 建立复方丹参片中三七定量显微鉴别方法,并改进异性有机物显微检查方法.方法 采用定量前处理,根据显微组织分布率计算三七投料情况;明确异性有机物的检查特征.结果 部分产品中三七未足量投料;排查了对异性有机物的误判可能.结论 采用植物组织分布率可初步判断三七投料是否足量;明确异性有机物检查特征保证了检测结果的准确可靠.     

Simultaneous analysis of 23 illegal adulterated aphrodisiac chemical ingredients in health foods and Chinese traditional patent medicines by ultrahigh performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry

This paper presents an application of ultra high-performance liquid-chromatography-quadrupole-TOF high resolution mass spectrometry (UHPLC-Q-TOF HRMS) for simultaneous analysis of 23 illegal adulterated aphrodisiac type chemical ingredients in health foods and Chinese Traditional Patent Medicines (CTPMs). The mass spectrometer was operated in Information Dependent Acquisition (IDA) mode, which provides crucial information for the elemental composition analysis, structure elucidation and quantitative analysis simultaneously. Quantitative analysis was performed using the peak areas of the precursor ions in the XICs. The method validation included assessment of selectivity, sensitivity, calibration curve, accuracy, precision, recovery, matrix effect and stability. The results show good linear relationship with the concentrations of the analytes over wide concentration ranges (e.g., 0.05–10 μg/g for sildenafil) as all the fitting coefficients of determination r² are >0.9984. The detection limits (LODs) were in the range of 0.002–0.1 μg/g. The recoveries were able to reach 82.5–103.6%, while the matrix effects ranged from 87.7 to 109.3%. The intra- and inter-day accuracies were in the range of 82.3–113.8%, while the intra- and inter-day precision ranged from 0.4 to 13.6%. Among 40 batches of health foods and 32 batches of CTPMs (including 28 capsules, 32 tablets, 10 liquid and 2 pills) samples, 28 batches of heath foods were positive. The detected chemical ingredients involved sildenafil, tadalafil, aildenafil and sulfoaildenafil. This method can be used for the screening, identification and quantification of illegal adulterated aphrodisiac chemical ingredients in health foods and CTPMs. Moreover, the LC-Q-TOF MS is very useful to structural elucidation of unknown compound.     

薄层色谱法测定降脂I号口服液中大黄酚的含量

目的：建立降脂I号口服液的质量控制方法。方法：薄层色谱法鉴别该中成药中的大黄素,大黄酚,大黄酸和大黄素甲醚,薄扫描法定量定大黄酚,结果：色谱板为硅胶H CMC－Na,展开剂正已烷－乙酸乙酯－甲酸（30：10：0．5）上层,薄层扫描波长434nm,大黄酚检测限为0.05ug,标准曲线Y＝4101,8X-1919(r=1.000),平均回收率99．77％,结论：所建立的方法特征性强,方法学考察满意,可作为降脂I号的质控方法。     

Number and size-spectra of myelinated nerve fibers of human premolars

Summary The primary objective of this study was to determine the number and size of myelinated nerve fibers at the subcervical, midroot and juxta-apical levels of human premolars. Sixty-seven healthy premolars extracted from adolescents were utilized. Root-discs were prepared from the three sites and processed for light and electron microscopy. The myelinated nerve fibers were counted from semithin sections using a sampling microscope. The measurements were taken from composite electron micrographs using an electronic image processing unit. A total of 1883 myelinated axons from seven mandibular second premolars was gauged. The 67 teeth had an average of 312±149 myelinated nerve fibers at the juxta-apical level (range 18 to 728). The contra- and ipsilateral differences in means among the four groups of premolars were not significant (P>0.05). The number of nerves increased significantly (P<0.05) toward midroot and subcervical (P<0.001) levels in all groups. The average neural diameter was 3.51.0 m at the juxta-apical level, and the between-teeth difference in mean was found to be significant (P<0.01). There was no decline (P>0.05) in the diameter of myelinated nerve fibers toward midroot and subcervical levels.     

Semiquantitative approach to CSF cytopathology

During the past two years, our laboratory has introduced a semiquantitative membrane filter approach to cerebrospinal fluid (CSF) cytology. Five hundred and thirty-five CSF specimens, averaging 3 ml in volume, were placed over 25-mm diameter Millipore filters (5-mu pore size) and stained using a modified Papanicolaou method. Each microscopic evaluation consisted of a cell count per milliliter, a 100-cell differential, and a diagnostic or interpretive statement. Seventy-four (13.8%) positive, 17 (3.2%) atypical, 439 (82%) negative, and 4 (1%) unsatisfactory specimens were evaluated. Seventy-four percent of the positive or atypical CSF specimens had mononuclear cell counts within the medically accepted normal range of five mononuclear cells per cubic millimeter (chamber count method) or 5,000 cells per millimeter (cytologic method). The small-filter technique offered advantages because it maximized cell retrieval, localized cells, and shortened the time required for microscopic evaluation.     

Patient variables impact lumbar spine dual energy X-ray absorptiometry precision

Introduction Changes in bone mineral density are used to monitor osteoporosis therapy. To determine whether a change in bone mass is clinically significant, the precision of bone mineral density measurements must be known. Methods We therefore measured the impact of vertebral body exclusion on dual energy X-ray absorptiometry (DXA) precision. At one university and one Veterans Affairs DXA center, three radiology technologists each scanned 30 participants twice, with repositioning between scans, to estimate DXA precision. Three International Society for Clinical Densitometry-certified physicians reviewed all lumbar spinal scans to note the presence of focal structural defects. We calculated precision for subsets of vertebrae, and for virtual samples of patients with and without physician-identified vertebral focal structural defects. We graphed the reciprocal of least significant change versus bone area to determine the dependence of precision on interpreted scan area. Results Within each sample, greater interpretable bone area improved precision. The contribution of interpreted bone area to precision differed among the samples, ranging from 57 to 94%. Greater population bone mineral density heterogeneity and presence of focal structural defects each decreased precision. Conclusion All bone densitometry centers must determine precision using a sample representative of their served populations. Failure to do so may lead to incorrect determination of least significant change. Population heterogeneity, vertebral body exclusion and presence of focal structural defects each decreases precision.     

脂蛋白X的定量分析及其在静脉营养支持中的应用

介绍一种简便、快捷的脂蛋白X的检测方法，通过乙醚提取脂蛋白X中磷脂，再经强酸消化后测定无机磷。对二组静脉输往脂肪乳剂的病例进行脂蛋白X监测，结果提示高磷脂／甘油三酯比例脂肪乳剂同时引起血清脂蛋白且和磷脂升高，脂蛋白X反映了机体对外源性磷脂的代谢情况。     

A hirudin catching ELISA for quantitating the anticoagulant in biological fluids

A catching ELISA has been developed that permits a quantitation of the anticoagulant hirudin in buffer, urine and plasma. In plasma hirudin can be determined in concentrations ranging from 0.2 to 25 ng/ml (2.4 × 10⁻³ to 0.3 AT-U/ml), in urine between 0.8 and 200 ng/ml (0.01 and 2.4 AT-U/ml). The enzyme immunoassay allows a rapid, sensitive and reproducible quantitation of hirudin, and can thus be used to assess the pharmacokinetics of the anticoagulant in patients after parenteral and/or topic administration.     

放射性核素在移植肾血管造影——血流灌注指数应用研究

为研究核素血管造影定量化分析指标——Hilson氏血流灌注指效在移植肾急性排斥反应的应用价值,本文报道了46只移植肾(正常对照28只,急性排斥18只)~(99m)Tc—DTPA肾血管造影定量分析结果,以该指数大于150或比正常基线检查增高25％为诊断标准,其灵敏性和特异性分别为88.9％和89.3％,抗排斥治疗后该指效明显下降。结果表明,该指标对急性排斥的诊断具有较高的灵敏性和特异性,且对抗排斥治疗效果观察具有意义。     

基因扩增检测四种感染人的疟原虫种类、数量的方法

目的建立对四种感染人的疟原虫种类、数量进行基因检测的方法。方法根据恶性疟、三日疟、卵形疟、间日疟的18SrRNA基因序列,设计属、种特异性引物和TaqMan探针,用荧光定量扩增反应确定标本中的基因拷贝数,用电泳区别各种疟原虫,并对2份疟疾血样进行检测。结果建立的检测方法对疟疾血样进行检测,荧光定量PCR具有良好的反应性,通过电泳能区分检测标本中的疟原虫株。结论建立的方法能够特异而灵敏地检测出标本中疟原虫的种类、数量,适合疟疾防治检测的需要。