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目的建立了一种高效液相色谱-三重四极杆串联质谱法,对氯沙坦钾原料药中遗传毒性杂质N-亚硝基-N-甲基-4-氨基丁酸(NMBA)进行测定。方法色谱柱为岛津Shim-pack XR-ODSⅡ色谱柱(2.0 mm×150 mm,2.2μm),流动相为0.1%甲酸水溶液(A)和甲醇(B),进行梯度洗脱,流速0.3 mL·min^-1,柱温为40℃,采用ESI离子化-三重四极杆质谱多反应监测(MRM)正离子模式检测,碰撞电压分别为-11,-13和-13 V,碰撞气氩气270 kPa,NMBA的离子对分别为m/z 147.15→117.10,147.15→87.10和147.15→44.10。结果该方法中NMBA在1~100 ng·mL^-1内线性关系良好,日内和日间的保留时间和峰面积的重复性良好(RSD均小于1.10%,n=6和n=18),低、中、高3个浓度的平均回收率在94.40%~98.04%之间。结论本方法简单方便,可快速有效的对氯沙坦钾原料药中NMBA进行限度检查并实现定量分析。  相似文献   
4.
生化自动分析仪在进行噪音核查和反应限核查之前,均已完成线性核查,已确定线性反应区,从吸光度-时间回归线计算出每分钟吸光度变化速度(△A/min)。在此基础上进行噪音核查(Noise Check)和反应限核查(Reaction Limit Check)。  相似文献   
5.
通过对冶金、锻造、铸造、陶瓷、纺织、印染、铁路、航运等行业的16个作业环境热环境参数和工人生理反应关系的调查,对现行的高温作业分级标准不足之处提出了一些看法,并认为IS0提出的热环境下机体反应的阈限值对我国亦是适宜的。经统计学分析发现,作业环境的计算温度和工人平均体温之间有明显相关(r=0.86)。不同气温下464名工人的主观感觉调查表明,35℃时100%的工人都有热或很热的感觉。  相似文献   
6.

Purpose

There is presently an ongoing debate on the relative merits of suggested criteria for spirometric airway obstruction. This study tests the null hypothesis that no superiority exists with the use of fixed ratio (FR) of forced expiratory volume in the first second (FEV1)/forced vital capacity (FVC) < 0.7 versus less than lower limit predicted (LLN) criteria with or without FEV1 <80% predicted in regards to future mortality.

Methods

In 1988–1994 the Third National Health and Nutrition Examination Survey (NHANES III) measured FEV1 and FVC with mortality follow-up data through December 31, 2011. For this survival analysis 7472 persons aged 40 and over with complete data formed the analytic sample.

Results

There were a total of 3554 deaths. Weighted Cox proportional hazards regression revealed an increased hazard ratio in persons with both fixed ratio and lower limit of normal with a low FEV1 (1.79, p < 0.0001), in those with fixed ratio only with a low FEV1 (1.77, p < 0.0001), in those with abnormal fixed ratio only with a normal FEV1 (1.28, p < 0.0001) compared with persons with no airflow obstruction (reference group). These remained significant after adjusting for demographic variables and other confounding variables.

Conclusions

The addition of FEV1 < 80% of predicted increased the prognostic power of the fixed ratio <0.7 and/or below the lower limit of predicted criteria for airway obstruction.  相似文献   
7.

Introduction

The usage of formalin-fixed paraffin embedded (FFPE) tissue is characterized by its long shelf-life and simple handling. Therefore it is the most commonly available tissue specimen in routine diagnostics and histological studies. Formaldehyde fixation may result in RNA degradation and cross linking with proteins, while storage conditions also affect RNA integrity. The present study was designed to investigate the influence of these factors on RNA analysis.

Design

FFPE-derived RNA from sections of 23 patients with spontaneous pneumothoraxes was used. Unstained sections of FFPE tissue were stored at various temperatures (?80?°C, ?20?°C, 4?°C, 24?°C) prior to RNA extraction. The potential impact on RNA quality of semi-automatic and manual RNA isolation and three different deparaffinization agents (mineral oil, xylene and d-limonene) were compared.

Results

The storage temperature of FFPE sections affects RNA concentration and fragmentation, with the optimal storage temperature below -20?°C. The RNA extracted with d-limonene shows equivalent quality to the RNA extracted using more toxic standard agents. The manual isolation provides a higher RNA yield compared to the semi-automatic isolation. However, no differences in the amount of longer RNA fragments were observed. Furthermore, the semi-automatic isolation showed an enhanced RNA quality.

Conclusion

FFPE sections not directly used for RNA extraction should be stored below -20?°C to increase quality and yield of the RNA. Usage of semi-automatic isolation produces superior results and simplifies routine processes by having less hands-on-time. Replacement of toxic xylene by d-limonene may contribute to improved occupational safety while not influencing analytical results.  相似文献   
8.
The series equivalent resistance R and capacitance C of metal/saline electrode/electrolyte interfaces were measured as a function of frequency (100 Hz–20k Hz) and current density (0·25 to 1000 A m−2) for eight typical electrode metals. For each of the metals tested, R decreased and C increased as the current density was increased above a critical value (with the exception of silver and MP35N at frequencies above 1 kHz for which R increased and C decreased slightly). With the exception of copper, the current density linearity limit (for 10 per cent decrease in R or 10 per cent increase in C) increased with increasing frequency and, in most cases, the current density linearity limit for 10 per cent increase in C was slightly less than that for 10 per cent decrease in R. Among the metals tested, copper and aluminium had the lowest current carrying capability and rhodium had the highest current-carrying capability. The current carrying capabilities of 316 SS, platinum, silver and MP35N, were intermediate and similar. With increasing current density, an increase in the electrode/electrolyte capacitance was the most sensitive indicator of the current-carrying linearity limit.  相似文献   
9.
A method for studying inhibitory activity in whole urine   总被引:4,自引:0,他引:4  
Summary A method has been developed for inducing and quantifying calcium oxalate crystallisation in whole human urine. The propensity of a given urine to induce crystal formation was described in two ways: 1) its ability to resist spontaneous nucleation of calcium oxalate crystals was assessed by titrating 20 mls of the urine with increasing quantities of sodium oxalate (0–150 mol) to determine its practical metastable limit. This limit was inversely related to the endogenous calcium concentration. 2) its capacity to inhibit crystal growth was quantified by determining the rate of growth of calcium oxalate crystals precipitated in response to a fixed oxalate load (30 mol) above its metastable limit. The crystals produced were predominantly calcium oxalate dihydrate and were morphologically identical to those occurring naturally in urine. Citrate had no effect on the metastable limits of 3 urines examined, but markedly inhibited crystal growth. Pyrophosphate had a similar effect on crystal growth, and in addition, raised the metastable limit of one of the urine samples.  相似文献   
10.
Twenty miles per hour (mph) speed limits can impact the health of the public (e.g., road safety, active travel). However, a better understanding of how individuals experience 20mph limits is required, to ensure interventions are cognisant of perceptions and potential un/intended outcomes. Focus groups (n = 9, 60 participants) to explore the Belfast 20mph intervention highlighted divergent perspectives and experiences including: 12 mechanisms (e.g., limited awareness), 15 pathways (e.g., reduced driving speed→improved liveability) and 10 public health outcomes (e.g., increased cyclist safety). Future interventions should consider un/intended outcomes and implement strategies to enhance effectiveness and mitigate harms (e.g., through training, enforcement).  相似文献   
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