分散固相萃取-超快速液相色谱-串联质谱法测定牛蛙全血中6种酚类环境雌激素

建立了一种快速、灵敏、准确的同时测定牛蛙全血中双酚A、己烯雌酚、己二烯雌酚、己烷雌酚、4-叔辛基酚和4-壬基酚等6种酚类环境雌激素的分散固相萃取-超快速液相色谱-串联质谱(dSPE-UFLC-MS/MS)分析方法。牛蛙全血样品经含0.1%(v/v)甲酸的甲醇溶液沉淀蛋白后,利用自制的氨基功能化Fe3O4磁性高分子复合微粒(EDA-MPs)作为dSPE吸附剂进行净化,着重考察了沉淀剂、吸附净化时间、吸附剂用量等因素对6种酚类环境雌激素回收率的影响。采用Shim-pack XR-ODSII(100 mm×2.0 mm, 2.2 μm)反相液相色谱柱进行分离,在电喷雾离子源(ESI)负离子多反应监测(MRM)模式下进行检测。结果表明: 6种酚类环境雌激素在0.5～100.0 μg/L范围内具有良好的线性关系(r2≥0.9996),方法的定量限(信噪比大于10)为0.075～0.40 μg/L,方法的精密度为0.6%～6.3%,空白样品中3个不同水平的添加回收率为95.0%～110.0%。本方法适用于牛蛙全血中6种酚类环境雌激素的同时测定。     

GC-FPD、GC-MS法分析血液样品中的毒鼠强

采用液-液提取方法及GC—FPD定量、GC—MS定性检测手段，对血液样品中毒鼠强的提取和检测方法进行了研究。时提取毒鼠强的溶剂类型、溶剂用量及质谱分析参数等因素进行了考察，建立了一种回收率高、重现性好、灵敏度佳、干扰少的毒鼠强分析方法。毒鼠强工作曲线的线性范围为0．01-0．2μg／μL，相关系数r=0．9999，空白血液的加标平均回收率为93．6％，测定结果的相对标准偏差为5．27％。该方法满足司法鉴定中生物样品的定性、定量检验要求。     

乌头碱的LC-MS定量分析

乌头生物碱各成分毒性差异很大,其中乌头碱的毒性为其它成分的100-2000倍,是引起中毒和死亡的主要原因。乌头生物碱种类多,在煎煮或泡制过程中易水解产生不同水解产物,进入体内后代谢情况又不明,因此采用液相色谱方法对体内检材乌头碱成分仅靠保留时间确定依据不足,定量工作更是无法开展。但在现实生活中炮制后的乌头植物可入药,且炮制过的乌头植物也可检出少量原碱。遇到体内检材中检验出乌头生物碱成分时,办案单位往往希望有一个量的甄别。经查阅资料,未见体内检材(如血、肝、尿等)中乌头碱含量的报道。我们应用LC-MS,采用646.4单离子扫描方式对实际案例血中乌头碱含量进行了测定,为今后的进一步研究和同行提供数据积累。     

兔VX2移植肝癌及隔离灌注模型建立方法探究

应用开腹瘤块包埋法建立了兔移植肝癌模型,探讨了改良动脉插管技术及提高隔离灌注模型建立的成功率.采用的方法是将实验兔建立移植肝癌模型10d后,按动脉插管方法随机分为3组：A组为直视下儿科静脉留置针插管;B组为显微镜下儿科静脉留置针插管;C组为直视下硬膜外麻醉导管插管.建模成功后经肝动脉灌注奥沙利铂,隔离灌注模型建立前测量肿瘤生长大小,常规病理观察肿瘤,比较插管成功率.研究结果表明：肿瘤生长良好,应用儿科静脉留置针插管成功率明显高于硬膜外麻醉导管,显微镜下插管较直视下无统计学意义,奥沙利铂浓度外周静脉显著低于流出道.由此认为采用儿科静脉留置针插管操作简单,成功率高,建立隔离灌注模型外周血药物泄漏少,阻断较完全,是一种实用的隔离灌注建立方法.     

红细胞分布宽度与心房颤动负荷的关系研究

目的观察病态窦房结综合征患者心房颤动负荷与红细胞分布宽度（RDW）的关系。方法选择病态窦房结综合征植入永久性人工心脏起搏器的患者81例,回顾性分析患者入院时基本资料、血常规及生化指标。记录术后3个月起搏器记录的心房颤动负荷。根据患者心房颤动负荷分为高负荷组及低负荷组,比较分析两组患者RDW及相关临床资料。结果心房颤动高负荷组患者RDW（15.61±1.23）%,高血压比例71%,明显高于低负荷组的（13.50±1.03）%、46%（P＜0.01或0.05）。高负荷组左心房直径、左心室舒张末期内径、WBC、TG、TC均大于低负荷组（P＜0.01或0.05）。心房颤动负荷影响因素的logistic回归分析显示,RDW是心房颤动负荷高的预测因素（OR=10.32,P＜0.01）。高TG、高血压、高胆固醇也是心房颤动高发的预测因素。结论心房颤动负荷除与年龄,高血压有关外,还与RDW明显相关。RDW可成为病态窦房结综合征患者心房颤动负荷的预测因素之一。     

功率谱和相关函数在脑血氧监测中的应用

采用自制的近红外双波长脑血氧监测仪实时采集人脑血和氧的数据，应用功率谱和相关函数的方法对采集的脑血氧的数据波形进行分析．结果发现正常人脑血氧波形之间有着严格的相关性，功率谱曲线主频峰清晰，血氧的功率谱曲线吻合好；脑缺氧病人血氧波形间的相关性差，功率谱曲线表现为主频峰不清晰，功率谱曲线吻合性差。临床试验表明：脑血氧波形、功率谱和相关函数对于分析人脑血、氧生理状况及其变化具有较好的效果。     

Determination of space‐dependent coefficients from temperature measurements using the conjugate gradient method

In this article, we consider coefficient identification problems in heat transfer concerned with the determination of the space‐dependent perfusion coefficient and/or thermal conductivity from interior temperature measurements using the conjugate gradient method (CGM). We establish the direct, sensitivity and adjoint problems and the iterative CGM algorithm which has to be stopped according to the discrepancy principle in order to reconstruct a stable solution for the inverse problem. The Sobolev gradient concept is introduced in the CGM iterative algorithm in order to improve the reconstructions. The numerical results illustrated for both exact and noisy data, in one‐ and two‐dimensions for single or double coefficient identifications show that the CGM is an efficient and stable method of inversion.     

动脉中血液脉动流的一种分析方法

动脉中的血液流动被分解为平衡状态(相当于平均压定常流状态)和叠加在平衡状态上的周期脉动流,利用Fung的血管应变能密度函数分析血管壁在平衡状态下的应力-应变关系,确定相对于平衡状态血管作微小变形所对应的周向弹性模量和轴向弹性模量,并建立在脉动压力作用下相应的管壁运动方程,与线性化Navier-Stokes方程联立,求得血液流动速度和血管壁位移的分析表达式,详细讨论血管壁周向和轴向弹性性质差异对脉博波、血液脉动流特性以及血管壁运动的影响.     

A projection method of estimation for a subfamily of exponential families

Summary This paper is concerned with estimation for a subfamily of exponential-type, which is a parametric model with sufficient statistics. The family is associated with a surface in the domain of a sufficient statistic. A new estimator, termed a projection estimator, is introduced. The key idea of its derivation is to look for a one-to-one transformation of the sufficient statistic so that the subfamily can be associated with a flat subset in the transformed domain. The estimator is defined by the orthogonal projection of the transformed statistic onto the flat surface. Here the orthogonality is introduced by the inverse of the estimated variance matrix of the statistic on the analogy of Mahalanobis's notion (1936,Proc. Nat. Inst. Sci. Ind.,2, 49–55). Thus the projection estimator has an explicit representation with no iterations. On the other hand, the MLE and classical estimators have to be sought as numerical solutions by some algorithm with a choice of an initial value and a stopping rule. It is shown that the projection estimator is first-order efficient. The second-order property is also discussed. Some examples are presented to show the utility of the estimator.     

Fluorescence assay of tyrosine in blood plasma

A more simple and sensitive assay for the quantitative determination of tyrosine in blood plasma is developed on the basis of a modification of the method of S. Udenfriend (1962). A volume of 0.2 ml of plasma is used in the analysis; after its deproteinization with trichloroacetic acid, it is reacted with sodium nitride, nitrous acid, and 1-nitroso-2-naphthol at 65°C, and the content of the reaction product is measured by the fluorescence at λ_ex/λ_em=460/570 nm. The consumption of plasma and reagents is reduced by a factor of 5–10 compared to the original method; in addition, the stage of extraction with an organic solvent is excluded. The linear dependence of the fluorescence signal on the tyrosine concentration within the range of 2–60 μg/ml, high specificity, accuracy, and reproducibility of the assay are shown. The importance of tyrosine determination in monitoring of glucocorticoid therapy and protein catabolism is discussed. Institute of Photobiology, National Academy of Sciences of Belarus, 27, Akademicheskaya St., Minsk, 220072, Belarus. Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 65, No. 3, pp. 366–371, May–June, 1998.