An LC-MS/MS method for creatine and creatinine analysis in paraquat-intoxicated patients

Abstract

A sudden increase in serum creatinine after paraquat intoxication has been reported in several clinical studies. However, this dramatic change of creatinine may be possibly due to an interconversion of creatine-creatinine in relation to paraquat toxicity. In order to investigate the creatine-creatinine relationship, a liquid chromatography tandem mass spectrometry in combination with electrospray ionization was developed and validated for simultaneous determination of creatine and creatinine in the serum. The chromatographic separation was achieved on a Gemini® C₆-Phenyl column with a gradient elution consisting of 0.1% formic acid in ultrapure water and methanol as the mobile phase. The method yielded suitable levels of specificity and selectivity, and calibration curves of creatine and creatinine in serum were linear over the concentration range of 0.5–200?µg mL^?1. The limit of quantification of both compounds was 0.5?µg mL^?1, and the method was accurate within the recovery range of 96.23–102.75%, indicating the robustness of the method. The method was successfully applied to toxicological samples from paraquat-intoxicated patients, and the concentrations of creatine and creatinine were quantified. High creatine concentrations in serum samples were observed which may lead to high serum creatinine despite normal kidney function as creatine is converted to creatinine in proportion to its concentration.     

气相色谱-串联质谱法测定沉积物中多环芳烃

采用ASE法提取沉积物中16种多环芳烃,以固相萃取法净化提取液,用气相色谱-串联质谱法测定。通过优化测定条件,使方法在5.00μg/L~1 600μg/L范围内线性良好,方法检出限为0.15μg/kg~0.66μg/kg。空白石英砂的加标回收率为61.9%~121%,7次测定结果的RSD为2.6%~11.1%。     

齐齐哈尔市PM2.5与PM10污染趋势及相关性分析

对2014—2016年齐齐哈尔市PM_(2.5)与PM_(10)质量浓度的时间变化特征进行简要分析,并探究PM_(2.5)/PM_(10)以及PM_(2.5)与PM_(10)的相关性。结果表明:2014—2016年齐齐哈尔的PM_(2.5)与PM_(10)的年均质量浓度分别为36.7、62.9μg/m~3,且呈逐渐下降趋势;冬季的PM_(2.5)与PM_(10)浓度最高,秋季次之,春季与夏季相对较低;2014—2016年PM_(2.5)与PM_(10)质量浓度月变化趋势基本相同,整体呈现2—6月逐渐下降,9—11月逐渐上升的规律;PM_(2.5)与PM_(10)质量浓度的日变化均呈双峰现象;对PM_(2.5)与PM_(10)进行线性拟合,相关系数为0.896 3。同时,残差分析也说明两者拟合情况良好,四季相关系数为r_(秋季)(0.982 2)r_(冬季)(0.964 4)r_(夏季)(0.943 9)r_(春季)(0.829 6);2014—2016年PM_(2.5)/PM_(10)平均值为55.27%,大气颗粒物PM_(2.5)的贡献率高达一半以上。     

溶解氧对好氧颗粒污泥影响的研究进展

好氧颗粒污泥技术是一种新颖废水处理技术。溶解氧(DO)是好氧颗粒污泥形成和稳定运行的一个重要参数。好氧颗粒污泥需要的曝气量大,能耗高。高曝气量带来的高DO浓度不利于氨氮通过SND去除。当DO扩散在颗粒内部受到限制时,颗粒中心形成的厌氧层不利于颗粒污泥的长期稳定运行。本文系统分析了DO浓度对好氧颗粒污泥影响的国内外研究现状,对好氧颗粒污泥中DO浓度这一重要参数的研究进行了总结。研究在低DO浓度下保持好氧颗粒污泥的稳定性有利于降低运行成本,采取合适的方法降低颗粒内部的扩散限制有利于增强颗粒的稳定性能。     

Determination of antibiotics in sewage from hospitals, nursery and slaughter house, wastewater treatment plant and source water in Chongqing region of Three Gorge Reservoir in China

Sewage samples from 4 hospitals, 1 nursery, 1 slaughter house, 1 wastewater treatment plant and 5 source water samples of Chongqing region of Three Gorge Reservoir were analyzed for macrolide, lincosamide, trimethoprim, fluorouinolone, sulfonamide and tetracycline antibiotics by online solid-phase extraction and liquid chromatography-tandem mass spectrometry. Results showed that the concentration of ofloxacin (OFX) in hospital was the highest among all water environments ranged from 1.660 μg/L to 4.240 μg/L and norfloxacin (NOR, 0.136-1.620 μg/L), ciproflaxacin (CIP, ranged from 0.011 μg/L to 0.136 μg/L), trimethoprim (TMP, 0.061-0.174 μg/L) were commonly detected. Removal range of antibiotics in the wastewater treatment plant was 18-100% and the removal ratio of tylosin, oxytetracycline and tetracycline were 100%. Relatively higher removal efficiencies were observed for tylosin (TYL), oxytetracycline (OXY) and tetracycline (TET)(100%), while lower removal efficiencies were observed for Trimethoprim (TMP, 1%), Epi-iso-chlorotetracycline (EICIC, 18%) and Erythromycin-H₂O (ERY-H₂O, 24%). Antibiotics were removed more efficiently in primary treatment compared with those in secondary treatment.     

Chemical and spectroscopic characterization of organic matter during the anaerobic digestion and successive composting of pig slurry

In this work, anaerobic digestion of pig slurry and successive composting of the digestate after centrifugation were studied by means of chemical analysis, FTIR and fluorescence spectroscopy as excitation–emission matrix (EEM). Chemical analysis highlighted the organic matter transformation occurring during the processes. A decrease of volatile solids and total organic carbon were observed in the digestate with respect to the fresh pig slurry as a consequence of the consumption of sugars, proteins, amino acids and fatty acids used by microorganisms as a C source. Water Extractable Organic Matter (WEOM) was obtained for all samples and fractionated into a hydrophilic and a hydrophobic fraction. The highest WEOM value was found in the pig slurry indicating a high content of labile organic C. The digestate centrifuged and the digestate composted showed lower hydrophilic and higher hydrophobic contents because of the decrease of labile C. Total phenolic content was lower in the digestate with respect to fresh pig slurry sample (36.7%) as a consequence of phenolic compounds degradation. The strong decrease of total reducing sugars in the digestate (76.6%) as compared to pig slurry confirmed that anaerobic process proceed mainly through consumption of sugars which represent a readily available energy source for microbial activity. FTIR spectra of pig slurry showed bands indicative of proteins and carbohydrates. A drop of aliphatic structures and a decrease of polysaccharides was observed after the anaerobic process along with the increase of the peak in the aromatic region. The composted substrate showed an increase of aromatic and a relative decrease of polysaccharides. EEM spectra provided tryptophan:fulvic-like fluorescence ratios which increased from fresh substrate to digestate because of the OM decompostion. Composted substrate presented the lowest ratio due to the humification process.     

宁波市大气可吸入颗粒物PM1o和PM2.5的源解析研究

在宁波市布设4个代表性点位,于2010年春季、夏季和冬季进行大气PM10和PM2.s的采样,同时采集了多种颗粒物源样品,建立了PM10、PM2.5和源样品的化学成分谱.采用化学质量平衡模型(CMB)对宁波市PM10、PM2.5进行源解析.结果表明,城市扬尘、煤烟尘、机动车尾气尘是宁波市PM10、PM2.5的3大污染源,...     

制药废水有机污染物特性分析与处理

分析了某制药企业废水生物处理站进出水中有机污染物的相对分子质量分布和气相色谱—质谱图谱,提出了根据废水水质特性有针对性地确定制药废水处理工艺的新思路.实验结果表明:进出水中的有机污染物主要是相对分子质量小于1 000的物质,且主要来源于车间5排放的COD比重大、水量小的工段废水;采用旋转蒸馏预处理法处理车间5废水,可使...     

Evaluation of photolysis and hydrolysis of pyraclostrobin in aqueous solutions and its degradation products in paddy water

This study evaluated the hydrolysis and photolysis kinetics of pyraclostrobin in an aqueous solution using ultra-high-performance liquid chromatography–photodiode array detection and identified the resulting metabolites of pyraclostrobin by hydrolysis and photolysis in paddy water using high-resolution mass spectrometry coupled with liquid chromatography. The effect of solution pH, metal ions and surfactants on the hydrolysis of pyraclostrobin was explored. The hydrolysis half-lives of pyraclostrobin were 23.1–115.5?days and were stable in buffer solution at pH 5.0. The degradation rate of pyraclostrobin in an aqueous solution under sunlight was slower than that under UV photolysis reaction. The half-lives of pyraclostrobin in a buffer solution at pH 5.0, 7.0, 9.0 and in paddy water were less than 12?h under the two light irradiation types. The metabolites of the two processes were identified and compared to further understand the mechanisms underlying hydrolysis and photolysis of pyraclostrobin in natural water. The extracted ions obtained from paddy water were automatically annotated by Compound Discoverer software with manual confirmation of their fragments. Two metabolites were detected and identified in the pyraclostrobin hydrolysis, whereas three metabolites were detected and identified in the photolysis in paddy water.     

Analysis of metabolic changes in Trichoderma asperellum TJ01 at different fermentation time-points by LC-QQQ-MS

Trichoderma spp. are among the most widely recognized biocontrol fungi used to inhibit pathogens and promote plant growth. These functions are related to primary and secondary metabolites. This study investigated the different metabolites in Trichoderma asperellum TJ01 cultured for 24 and 72?h using liquid chromatography with triple-quadrupole mass spectrometry. Compared to the 24?h culture of T. asperellum TJ01, the 72?h culture with amino acid metabolism tended to decrease while sugar and lipid metabolisms tended to increase. Furthermore, the 72?h culture had a higher proportion of upregulated flavonoids, in combination with a higher proportion of downregulated alkaloids, and equal proportions of upregulated and downregulated polyphenols and hormones. This study also identified a few valuable medicinal substances such as trigonelline and 5-hydroxytryptophan in T. asperellum TJ01 fermentation cultures.