直接进样-高效液相色谱-串联质谱分析水中微囊藻毒素

建立了直接进样-高效液相色谱-串联四极杆质谱分析环境水样中微囊藻毒素-LR的分析方法。方法使用C18反相柱为分离柱,柱温40℃,流速0.7 mL/min,乙腈和甲酸水溶液(0.1%)作流动相,采用梯度洗脱,保留时间4.13 min。串联质谱采用多反应监测模式,使用ESI(+)源电离水样。在上述条件下,水样过粒径为0.45μm的滤头后可直接进样,进样体积25μL时检出限可达0.04μg/L,在0.10~200μg/L范围内线性良好(R=0.999 8);样品加标回收率为96.6%~106%,相对标准偏差为1.3%~5.6%。同时方法应用到实际环境水样分析中也具有令人满意的结果。该方法灵敏度高,快速简单,适用于环境水样中MC-LR的分析。     

固相萃取-气相色谱法测定水样中马拉硫磷残留

采用C-18小柱萃取、毛细管柱分离、气相色谱氢火焰离子化检测器（FID）测定水样中的马拉硫磷,检测限为0．12μg／L。试验了样品流量和洗脱剂对回收率的影响,结果表明样品流量为6mL／min、二氯甲烷作洗脱剂时,回收率较好。测定蒸馏水、地下水和河水样品,相对标准偏差〈2．2％。加标回收率在79．0％-109％之间。     

Characterization of distribution of pesticide residues in crop units

The characteristic features of distribution of pesticide residues in crop units and single sample increments were studied based on more than 19,000 residue concentrations measured in root vegetables, leafy vegetables, small-, medium- and large-size fruits representing 20 different crops and 46 pesticides. Log-normal, gamma and Weibull distributions were found to provide the best fit for the relative frequency distributions of individual residue data sets. The overall best fit was provided by lognormal distribution. The relative standard deviation of residues (CV) in various crops ranged from 15–170%. The 100–120 residue values being in one data set was too small to identify potential effects of various factors such as the chemical and physical properties of pesticides and the nature of crops. Therefore, the average of CV values, obtained from individual data sets, were calculated and considered to be the best estimate for the likely variability of unit crop residues for treated field (CV = 0.8) and market samples (CV = 1.1), respectively. The larger variation of residues in market samples was attributed to the potential mixing of lots and varying proportion of non-detects. The expectable average variability of residues in composited samples can be calculated from the typical values taking into account the sample size.     

环境生物样品预处理中的微波溶样技术

微波溶样是近年产生的一种崭新的有前途的样品预处理技术，本文评述这一技术在环境、生物样品消解方面的近期应用。     

广州市在用机动车排气抽检工作若干问题探讨

介绍了广州市在用机动车抽检工作情况和程序,分析了排气抽检工作中存在的问题,提出了解决问题的建议和方法。     

类固醇雌激素分析方法研究进展

类固醇雌激素因其对野生动物、人类健康及生态环境安全造成危害而受到全世界的普遍关注,并成为环境科学和生态毒理学研究的重点和热点之一.针对4种典型的类固醇雌激素(雌激素酮、17-β-雌二醇、雌三醇和17-α-乙炔基雌二醇),对其羟基和酮基衍生化技术、水和固体样品的前处理技术及仪器检测方法进行了综述,总结了类固醇雌激素分析方法的研究动态和进展.     

QuEChERS: a sample preparation for extraction of carbaryl from rat feces

Carbamate compounds are an important group of cholinesterase inhibitors. There is a need for creating awareness regarding the risks of the inadequate carbamate use in the residential areas due to potential adverse human effects. Carbaryl is a commonly used pesticide worldwide. A simple, fast, and high-throughput method was developed employing liquid chromatography with fluorescence detector to determine carbaryl residues in rat feces. The extraction was performed by using a rapid, easy, cheap, effective, reliable, and safe (QuEChERS) method, using acetonitrile as the extracting solvent. The parameters for the performance of the extraction method were optimized, such as ratio of mass of sample per volume of extraction solvent, QuEChERS content, and cleanup columns. Linear response was obtained for all calibration curves (solvent and matrix-matched) over the established concentration range (5–500 μg/L) with a correlation coefficients higher than 0.999. The achieved recovery was 97.9% with relative standard deviation values of 1.1% (n = 4) at 167 μg/kg fortified concentration level and the limits of detection and quantification were 27.7 and 92.3 µg/kg, respectively.     

低水平放射性废水中钚的分析方法研究进展

钚是重要的核燃料,也是一种极毒的放射性核素,在核燃料循环和放射性废物处置过程中占有重要地位.近些年来,钚在自然水体中的含量、分布引起人们的关注.科研工作者针对低水平放射性废水,核设施周围自然水体,核试验、核事故情况下可能污染的自然水体等,建立了一些钚的分析方法.作者在对这些方法进行了比较的基础上,提出了一种在盐酸体系中用TEVA树脂负压微色谱柱液闪法将水溶液中钚与其他锕系元素及金属离子分离并测量的新方法.该方法有望在日常和应急监测中的得到应用.     

通过屋顶暴露方法模拟聚碳酸酯微塑料在长江水样的长期老化行为

由于较低的自然老化速率,微塑料在实际水体长期户外暴露过程中老化行为的数据仍较缺乏.通过聚碳酸酯（Polycarbonate,PC）微塑料在长江表层水样的18个月户外暴露试验以揭示自然老化过程对微塑料表面特征及对金属离子(Cr⁶⁺和Co²⁺)吸附行为的重要影响.结果显示,户外暴露改变了PC微塑料的理化性质,包括表面开裂、粒径降低、亲水性和熔点增加以及表面氧化（产生羰基和羟基）.同时,户外老化过程明显影响微塑料对金属离子的吸附行为.原始和低老化程度PC对金属离子的吸附主要通过物理作用控制,而高老化程度微塑料由于产生含氧功能团对金属离子的吸附主要由化学过程如络合和共价键等作用控制.并且,不同老化程度PC微塑料对Cr⁶⁺和Co²⁺的吸附性能不同.对于Cr⁶⁺,PC的吸附性能随其老化程度增加呈先升高后降低的趋势,然而对于Co²⁺,平衡吸附性能随老化程度增加呈增加的趋势.户外老化过程产生含氧官能团、破碎和开裂以及生物膜可能是影响吸附性能的主要因素.本研究证实了长期户外...     

战斗部飞行可靠性评估方法研究

目的 解决高可靠、小子样战斗部飞行可靠性评估时样本量不满足标准要求的问题。方法 通过对战斗部结构功能分析,建立包含壳体强度、主装药安定性及主装药正常起爆等单元的可靠性框图,并利用L-M法对战斗部系统进行可靠性评估。首先利用基准设计许用值的安全系数法将应力强度干涉模型与安全系数进行结合,对壳体强度可靠性进行评估;然后结合战斗部试验数据,利用最大熵试验法,在小样本下评估战斗部主装药安定性及正常起爆的可靠性;最后,将各单元的可靠性数据转化为成败型数据进行分析,利用L-M法,结合战斗部整机试验数据,开展战斗部飞行可靠度评估。结果 分别计算了小子样下战斗部壳体和装药安定性及正常起爆的可靠度,并将其转换为等效成功数和等效失败数,结合战斗部试验打靶等可靠性信息,综合评估了战斗部飞行可靠度。结论 充分利用战斗部在研制阶段的试验信息进行评估,减少了样本量,解决了战斗部可靠性高、样本量小的评估难题。