Development and validation of LC-MS/MS method for the determination of Ochratoxin A and its metabolite Ochratoxin α in poultry tissues and eggs

The objective of this study was to develop a liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the determination of Ochratoxin A (OTA) and Ochratoxin α (OTα) in poultry tissues and eggs. The two toxins were extracted by a mixture of acetonitrile/water, purified with a reversed phase C18 solid phase extraction column (SPE) and determined by LC-MS/MS. The LC-MS/MS method performances were evaluated in terms of linearity in solvent and in matrix (ranged from 0.5 to 15.10 µg L^?1 for OTA and from 0.60 to 17.85 µg L^?1 for OTα), limit of detection (LOD), limit of quantitation (LOQ), specificity, accuracy and precision in repeatability conditions. Recovery experiments were performed by spiking poultry liver, kidney, muscle and eggs around 1 µg kg^?1 and 10 µg kg^?1. LODs were 0.27 and 0.26 µg kg^?1 while LOQs were fixed at 1.0 and 1.2 µg kg^?1 for OTA and OTα, respectively. Main recoveries for OTA ranged from 82 to 109% and for OTα ranged from 55 to 89%. The values of within-laboratory relative standard deviation (RSD_r) were equal to or below 20%. Considering the results obtained and that all analytical performance criteria were fulfilled, the new extraction and purification method developed for OTA and OTα determination in animal tissues and eggs was found appropriate for control laboratories and research activities designed to ensure food safety.     

环境空气自动监测方法检出限相关问题探讨

探讨了环境空气自动监测中实际评估方法检出限的意义,详细介绍了常规气态污染物自动监测方法检出限的评估方法。并以EC 9850型SO2分析仪为例,说明了环境空气自动监测的测定步骤和方法检出限的计算。     

两种吹扫捕集浓缩仪在测定土壤VOCs时的性能比较

从仪器精密度、方法检出限、准确度等角度对吹扫捕集浓缩仪Stratum PTC与Eclipse 4660的性能进行比较。结果表明,大部分分析物用Stratum PTC的方法检出限略高于Eclipse 4660,但精密度比Eclipse 4660稍差;Eclipse 4660用于分析极性的、水溶性物质的效果比Stratum PTC好,回收率更高。两种吹扫捕集仪的测试结果均满足《土壤和沉积物挥发性有机物的测定吹扫捕集/气相色谱-质谱法》(HJ 605-2011)标准方法的指标要求。     

探究土壤中萘提取液的浓缩方法比较

随着科学技术的发展,工业产品越来越丰富。工业工艺过程、缺氧燃烧、垃圾焚烧和填埋等生产活动,产生了大量的多环芳烃物质。这些物质通过复杂的物理迁移、化学及生物转化反应,进入土壤,严重污染环境,给人类及其生物的安全带来严重危害。如何快速、准确检测土壤中多环芳烃的含量,成为治理污染等相应策略实施的首要条件。当前测定土壤中多环芳烃的前处理方法有加压流体萃取、索式萃取、超声波萃取、微波萃取等。在这些成熟萃取手段中,浓缩又是一个关键步骤。目前浓缩的手段有KD浓缩、氮吹浓缩、旋转蒸发浓缩、旋转与氮吹合用浓缩。本文对四种浓缩手段对多环芳烃中的萘提取液进行浓缩分析比较,并获得了一定结论,望给行业内提供有效的参考意见。     

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.     

便携β射线法手工监测PM_(2.5)的可行性研究

提出利用自动射线原理结合重量法的简捷便携特点的便携射线仪手工监测PM2.5的思路,平行比对了便携射线法和手工重量法所测60组PM2.5浓度的监测结果,采用线性回归及T检验、F检验等理论分析了两者数据结果间的有效性和可比性。结果表明,便携式射线仪监测结果与重量法监测结果之间有效可比且得到了两者间的线性回归方程;此外进行了20组数据的实样验证,换算值和真值之间相对误差在8%以内,因而确定了便携射线仪手工监测PM2.5的可行性。     

纳污湿地上覆水中重金属的监测及评价

以武河湿地为研究区域采集上覆水水样,采用ICP-AES法测定湿地水体中重金属的含量,参照有关标准用水质标准级别法对水中重金属污染情况进行了评价。结果表明:武河湿地中重金属Hg污染十分严重,各采样点均有分布且水质属劣Ⅴ类。重金属元素Cd污染并不严重,总体水质较好。重金属元素As、Cr、Cu、Pb在武河湿地中污染较轻近乎无污染,水质为Ⅰ类。由于重金属Hg的污染十分严重所以研究区内综合质量等级在4以上,水质为Ⅴ类和劣Ⅴ类,污染严重。     

Physiologically based pharmacokinetic modeling of perfluoroalkyl substances in the human body

Currently, there are limited data on the levels of perfluoroalkyl substances other than perfluorooctane sulfonic acid and perfluorooctanoic acid in the human body. Most of this information has been extracted from biological monitoring of plasma while the occurrence of perfluoroalkyl substances in other human tissues is rarely studied. The objective of the present study was to develop a physiologically based pharmacokinetic model to assess the concentration of perfluoroalkyl substances in human tissues, based on an existing model previously validated for perfluorooctane sulfonic acid and perfluorooctanoic acid. Experimental data on concentrations of perfluoroalkyl substances in human tissues from individuals in Tarragona County (Catalonia, Spain) were used to estimate the values of some distribution and elimination parameters needed for the simulation. No significant correlations were found between these parameters and the chain lengths. The model was finally validated for five perfluoroalkyl substances.     

关于重量法测定硫酸盐化速率的不确定度分析

碳酸钾溶液浸渍过的玻璃纤维滤膜曝露于空气中,与空气中的二氧化硫、硫酸雾、硫化氢等发生反应,生成硫酸盐。测定生成的硫酸盐含量,计算硫酸盐化速率。不确定度的来源主要包括:样品重复性分析、电子天平称量等。评定结果为硫酸盐化速率的不确定度(2.90±0.06)(SO3),mg/(100cm2碱片·d),k=2。     

TRMM降水数据在东北地区的精度验证与应用

利用东北地区2000—2007年的APHRODITE降水数据,基于GWR方法对TRMM降水数据进行修正,分析新的TRMM降水数据精度,并基于修正的TRMM降水数据对东北地区降水进行时空分布特征分析。结果表明:1APHRODITE降水数据与观测数据之间的线性相关性更高、均方根误差RMSE更小,数据具有较高的精度;2修正后的TRMM降水数据相关系数R有所提高,且RMSE值均有降低。整体来看,TRMM降水数据的降水量数值偏大于观测值;3修正TRMM降水数据在5—10月的误差相对较小,整体来看,在大部分区域的误差在0~30%之间;4东北地区降水分布极不均匀,整体呈从东南向西北减少趋势。11月到翌年3月的降水稀少,降水主要集中在夏季,其中7月降水量最大。