LC-MS/MS法测定比格犬血浆中的阿那曲唑

用高效液相色谱-串联质谱法(LC-MS/MS)测定比格犬血浆中阿那曲唑的浓度。以苯磺酸氨氯地平为内标,加入50μL血浆,用甲基叔丁基醚萃取后取上清液以氮气吹干,用50%甲醇水溶液复溶,进样5μL,在电喷雾离子源下进行正离子检测。色谱柱为Agilent XDB C18(50mm×2.1mm×3.5μm),流动相为0.1%甲酸水-0.1%甲酸乙腈(60∶40)。阿那曲唑和内标的质荷比(m/z)分别为294.4和409,阿那曲唑和内标生成的主要碎片离子的质荷比(m/z)分别为255.3和238。阿那曲唑在0.5~500 ng·mL-1内线性良好,检出限为0.5ng·mL-1,提取回收率均大于80%,日内、日间准确度为101%~104%,日内、日间精密度分别小于7.04%和8.69%,已成功检测比格犬血浆中阿那曲唑的血药浓度。所用方法稳定、灵敏度好、分析时间短、提取回收率高,适用于比格犬血浆中阿那曲唑的血药浓度测定。     

UPLC-MS/MS测定人血浆中罗红霉素的浓度及在药代动力学中的应用

建立一种快速、准确测定人血浆中罗红霉素浓度的UPLC-MS/MS分析方法。以克拉霉素为内标,0.2mL含药血浆经碱化、乙酸乙酯萃取后进样分析;色谱柱为Acquity UPLC BEH C18（2.1mm×50mm×1.7μm）,流动相组成为乙腈∶0.01%醋酸铵=30∶70,梯度洗脱方式,乙腈比例在4 min内从30%变为70%,流速0.3 mL/min,柱温为35℃,进样量3μL。质谱条件：气动辅助电喷雾离子化（ESI）源;正离子检测（MRM）模式,罗红霉素质荷比为（m/z 837.53→m/z 158.15）和克拉霉素质荷比为（m/z 748.48→m/z 590.30）。罗红霉素在0.05~25.6μg/mL的浓度范围内呈线性,定量下限为0.05μg/mL,基质效应影响小,日内变异系数小于10.3%,日间变异系数小于9.4%,相对回收率在97.5%~106.4%之间。该方法准确、快速、灵敏,可用于微量血浆的罗红霉素药物浓度监测、人体内药代动力学及生物等效性研究。     

LC-MS/MS法测定Beagle犬血浆中ET-26盐酸盐及其代谢产物ET-acid

该文通过建立LC-MS/MS方法,采用全扫描离子(MRM)检测方式,测定静脉注射给药后Beagle犬中ET-26盐酸盐及其代谢产物依托咪酯酸的含量。采用色谱柱Agilent Extend-C18(3.0 mm×100 mm,3.5μm),流动相为水(0.01%NH3,用乙酸调pH至9.0)-乙腈,体积比35:65,采用ESI离子源,正离子模式下定量分析碎片离子质荷比(m/z)有ET-26盐酸盐275.3/105.1,依托咪酯酸m/z 217.0/113.1,依托咪酯杂质C(内标)m/z 259.0/155.1。ET-26盐酸盐与依托咪酯酸分别在3.225~2 090 ng/mL、3.253~2 108 ng/mL范围内,线性关系良好;定量限分别为3.225 ng/mL、3.253 ng/mL;检测限分别为0.97 ng/mL、1.00 ng/mL;日内、日间精密度RSD均小于15%;回收率分别在86.57%~105.03%、95.94%~98.27%范围内。该方法成功应用于Beagle犬中ET-26盐酸盐的药代动力学参数测定。结果表明该方法可以灵敏、有效地测定Beagle犬血浆中ET-26盐酸盐及其代谢产物依托咪酯酸的含量。     

HPLC-MS/MS法同时测定人血浆中奥美拉唑及其代谢物

建立HPLC-MS/MS法测定人血浆中奥美拉唑(OPZ)及代谢物奥美拉唑砜(S-OPZ)、5-羟基奥美拉唑(HOPZ)的浓度,以用于奥美拉唑的药代动力学研究。采用Phenomenex Gemini C18(50 mm×3.0 mm,5μm)色谱柱,乙腈-水(体积比40∶60)为流动相,流量0.2 m L/min,以d3-奥美拉唑(d3-OPZ)作内标,血浆样本用二氯甲烷∶异丙醇(体积比97∶3)萃取,采用ESI源,正离子MRM模式检测。OPZ在0.5~600 ng/m L范围内,S-OPZ和H-OPZ在0.25~300 ng/m L范围内线性良好;OPZ、S-OPZ、H-OPZ及IS的保留时间分别为3.19,4.18,1.96,3.19 min左右;萃取回收率在53.8%~84.6%;高浓度血浆样品稀释4倍测定不影响结果 ;精密度、基质效应经内标校准后均合格;稳定性各项数据均符合相关要求。该法快速、灵敏、专属性强、重现性好,适用于奥美拉唑及其代谢物的血药浓度测定。     

UPLC-MS/MS法同时测定人血浆中氯沙坦及其代谢物浓度

建立UPLC-MS/MS法测定人血浆中氯沙坦及代谢物氯沙坦羧酸的浓度,以用于氯沙坦的药代动力学研究。采用Sepax GP-C18(2.1 mm×50 mm,1.8μm)色谱柱,以0.15%甲酸-0.04%氨水-水(超声20 min后,加入0.01%氨水)为水相,0.15%甲酸-0.04%氨水-98%乙腈为有机相。梯度洗脱,流量为0.3 mL/min。以d4-氯沙坦、d4-氯沙坦羧酸作内标,血浆样本用乙腈一步沉淀蛋白,采用多反应离子监测,正离子模式扫描,电喷雾离子源。结果表明:氯沙坦在2.0~2 000 ng/mL范围内,氯沙坦羧酸在2.4~2 400 ng/mL范围内线性良好;氯沙坦及内标的保留时间为1.16 min左右,氯沙坦羧酸及内标的保留时间为1.26 min左右;氯沙坦、氯沙坦羧酸提取回收率分别为109.9%、97.55%;精密度、基质效应经内标校准后均合格;稳定性各项数据均符合相关要求。该法快速、灵敏、专属性强、重现性好,适用于氯沙坦及其代谢物的血药浓度测定。     

UPLC-MS/MS同时测定人血浆中替米沙坦与氨氯地平浓度

建立UPLC-MS/MS法同时测定人血浆中替米沙坦与氨氯地平的浓度,用于研究替米沙坦/氨氯地平片的药代动力学。采用Waters BEH C18 (2.1 mm×50 mm,1.7μm)色谱柱,流动相A:甲酸∶氨水∶水(1∶0.2∶1 000,v/v/v),流动相B:甲酸∶氨水∶乙腈∶水(1∶0.2∶950∶50, v/v/v/v),进行梯度洗脱,流量0.3 mL/min,以d3-替米沙坦、d4-氨氯地平作内标。血浆样本液液萃取后,采用SHIMADZU SIL-30 AD型UPLC进样分离,美国AB Sciex QTRAP 5500质谱仪在MRM模式下检测。结果表明:替米沙坦在0.50～500 ng/mL范围内,氨氯地平在0.05～8.00 ng/mL范围内线性良好;替米沙坦及内标的保留时间均为1.43 min,氨氯地平及内标的保留时间均为1.31 min;替米沙坦萃取回收率103.0%～104.2%、氨氯地平萃取回收率54.6%～66.5%;方法的特异性、灵敏性、线性、精密度、准确度、基质效应以及稳定性验证数据均符合相关要求。该法快速、灵敏、专属性强、重现性好,适用于替米沙坦/氨氯地平的血药浓度测定。     

LC-MS同时测定大鼠脑脊液中谷氨酸和γ-氨基丁酸的方法研究

建立LC-MS同时检测大鼠脑脊液中谷氨酸和γ-氨基丁酸的方法。采用安捷伦ZORBAX SIL(4.6 mm×250 mm×5μm)硅胶正相色谱柱,流动相为甲醇-水(0.1%甲酸)=50∶50(v/v),梯度洗脱,流速为1 m L/min。电喷雾离子源(eletrospray ionization,ESI)采用正离子化方式,以多重反应检测(multiple reaction monitoring,MRM)方式进行检测,用于定量分析的离子反应分别为m/z 148.1→m/z 84.1(谷氨酸,[M+H]+),m/z 104.1→m/z 87.1(γ-氨基丁酸,[M+H]+)。测定大鼠脑脊液中谷氨酸在500~2 500μg/L和γ-氨基丁酸在50~250μg/L质量浓度范围内,浓度与峰面积呈良好的线性关系。该方法简便、准确、灵敏度高,专属性强,重复性好,适用于脑脊液中谷氨酸和γ-氨基丁酸的同时测定,可为氨基酸类神经递质提供有效的检测手段。     

UPLC-MS/MS法快速检测保健食品中非法添加西地那非等化学药物成分

建立UPLC-MS/MS测定保健食品中非法添加西地那非及其类似物的检测方法。应用Waters xevo TQD液质联用仪超高效液相色谱C18柱(100X2. 1mm,1. 7!m)分离,流动相:0. 1%甲酸乙腈(A):0. 1%甲酸水溶液(B) 20:80梯度洗脱,流速:0. 3mL/min,进样量:10μL,柱温:30℃;采用ESI电离子源正离子源模式,取他达拉非m/z母离子390. 4,子离子135. 1、268. 0;西地那非m/z母离子475. 1,子离子283. 1、311. 1,伐地那非m/z母离子489. 3,子离子312. 2、151. 1,硫代艾地那非m/z母离子505. 2,子离子99. 0、113. 1,羟基豪莫西地那非m/z母离子505. 2,子离子99. 0、112. 0,伪伐地那非m/z母离子460. 2,子离子151. 1、312. 2,那红地那非m/z母离子453. 2,子离子97. 1、113. 0,作为定量目标离子进行检测。结果表明:以上7种化学成分进样量10!L,在上述色谱条件和质谱条件下5min内得到快速分离,且分离度较好,线性范围宽,在10～100ng/m L的线性氛围内相关系数r均大于0. 998,回收率在81. 8～109. 1%,精密度RSD为1. 2～3. 3%。本方法通用性强,操作简单,快速,检测结果精准,可作为保健食品中非法添加西地那非等化学成分的快速定性定量的检测方法。     

柱前衍生化反相高效液相色谱法测定大鼠血浆中牛磺酸的含量及其药动学研究

建立一种测定大鼠血浆中牛磺酸含量的柱前衍生化-高效液相色谱法,并将其应用于牛磺酸在大鼠体内的药动学研究。采用柱前衍生化高效液相色谱法,以2,4-二硝基氟苯(DNFB)为衍生化试剂,以KH2PO3缓冲液(pH7.0):乙腈∶水(70∶15∶15,v/v)为流动相,经C18色谱柱(250mm×4.6mm×5μm)分离,柱温30℃,流速1.0m L/min,进样量为20μL,牛磺酸衍生物的紫外检测波长为360 nm,并以DAS2.0计算其药动学参数。大鼠血浆中牛磺酸在1.29~1 287.5μg/m L质量浓度范围内线性关系良好,r=0.999 9,最低定量限1.29μg/m L,主要药动学参数t1/2为(3.747±1.430)h,Cmax为(949.573±192.967)μg/m L,Tmax为(1.000±0.000)h,AUC0-t为(2 862.168±565.917)(mg/L)/h。该法简单、经济、灵敏,适用于牛磺酸血药浓度测定及药动学研究。     

阿哌沙班中8种已知杂质的HPLC法定量检测

建立高效液相色谱法测定阿哌沙班中的8个已知杂质。色谱柱为Waters Xbridge Shield RP18(150mm×4.6mm,5μm);以乙腈-醋酸铵溶液为流动相,柱温:40℃,流量:1.0 m L/min,检测波长280 nm。阿哌沙班中8种杂质分离较好,与主峰均能有效分离,线性范围为0.01~11μg/m L;8种杂质的平均回收率分别为98.7%,105.3%,100.7%,111.4%,97.4%,103.4%,98.9%,97.6%,RSD分别为2.8%,4.3%,3.3%,4.5%,3.1%,4.0%,2.7%,3.1%。该法简便、准确、重复性好,可为阿哌沙班质量标准的制定提供参考。     

Gender differences in publication productivity in psychology in India

An analysis of gender differences in psychology in India provides quantitative and qualitative assessment of R&D output contributed by psychologists with the indication of the trend of growth, skewness, relatedness, co-authorship pattern of productivity.     

Metrology in Chemistry in Germany

The system for Metrology in Chemistry in Germany is described. At the national standards level, a network of high-level chemistry institutes coordinated by the national metrology institute, PTB, provides the primary references for chemical measurements. A dissemination mechanism employs chemical calibration laboratories accredited within the framework of the German Calibration Service (DKD). They act as “multipliers” between the national standards level and the user level by providing the user with calibration means which are traceable to the SI via national standards. Traceability structures in clinical chemistry, electrochemistry, elemental analysis and gas analysis are described     

Natural radioactivity in drinking water in private wells in Finland

Natural radioactivity in drinking water was determined in population-based random study of 472 private wells. The mean concentrations of (222)Rn, (226)Ra, (234)U, (238)U, (210)Pb and (210)Po in drilled wells were 460, 0.05, 0.35, 0.26, 0.04 and 0.05 Bq l(-1), and in wells dug in the soil were 50, 0.016, 0.02, 0.015, 0.013 and 0.007 Bq l(-1), respectively. Approximately 10% of the drilled wells exceeded a radon concentration of 1000 Bq l(-1) and 18% a uranium concentration of 15 microg l(-1). The mean annual effective dose from natural radionuclides for a drilled well user was 0.4 mSv and 0.05 mSv for a user of a well dug in the soil. The effective dose arising from (222)Rn was 75% of the total of all natural radionuclides for drilled well users. As regards long-lived radionuclides, (210)Po and (210)Pb caused the largest portion of the effective dose. The dose arising from (238)U, (234)U and (226)Ra was only 8% of the total of all natural radionuclides.     

Natural radioactivity in drinking water in private wells in Finland

Radiation Protection Dosimetry     

Optische in situ Schichtdickenmessung in Bedampfungsanlagen. Optical in situ film thickness monitoring in coating systems

Optical film thickness monitoring is more precise than crystal monitoring. The optical measurement makes use of the fact that the intensity of a monochromatic light beam which is reflected on a film will change periodically with increasing film thickness. The measurement is performed at an exchangeable test glass that is positioned beside the substrates and is therefore coated in the same way as the substrates. The accuracy of cut‐off is achieved by a “fit” of a theoretical curve shape to the measured values. Order filters are used to ensure that, at a certain wavelength, higher deflection orders do not influence the measurement when a monochromator grating is used.     

Spanish experience in education and training in radiation protection in medicine

In most of its publications, the International Commission on Radiological Protection has highlighted the importance of education and training in radiation protection (RP) for medical exposures. Spain, like other Member States of the European Union, has implemented the Directive and the Guidelines in the medical area. The purpose of this paper is to present the Spanish experience in RP education and training in medicine, the different objectives established according to professional levels, existing regulations and feedback obtained from various RP actions.     

Differences in coagulation in clotting of vascular access in hemodialysis patients

Arteriovenous graft (AVG) thrombosis is a frequent cause of graft failure. We evaluated coagulation protein concentrations, platelet function, and viscoelasticity factors in 20 hemodialysis (HD) patients with AVGs. The goal was to determine whether significant differences in protein concentrations, platelet function, and viscoelasticity factors exist among dialysis patients requiring frequent AVG declot procedures vs. those who do not. Twenty HD patients were enrolled: 10 frequent clotters (>3 declots in the previous year) and 10 were nonclotters. Patients on antiplatelets or chronic anticoagulation were excluded. Laboratories were drawn pretreatment and heparinase was added to counteract any potential heparin effect. Coagulation protein concentrations including tissue factor (TF), thrombin/antithrombin III complex (TAT), and prothrombin fragment 1 + 2 (F₁₊₂) were assayed. The time to clot onset was measured by force onset time (FOT). Platelet contractile force (PCF) measured the force produced by platelets during clot retraction, whereas clot rigidity was measured as clot elastic modulus (CEM). FOT, CEM, and PCF were measured by Hemodyne. Both groups had upregulation of the TF pathway, as TF, TAT, and F₁₊₂ levels were similarly increased over baseline levels. Hemodialysis patients with frequent AVG clotting had higher levels of both PCF and CEM compared with nonclotters. Additionally, the frequent clotters had a lower FOT relative to nonclotters, although both were considered in the normal range. Our study suggests that HD patients with recurrent AVG thrombotic events form clots with higher tensile strength compared with HD patients without recurrent graft thrombosis.