水浴磁力搅拌碱消解-火焰原子吸收分光光度法测定土壤中铬（Ⅵ）

建立水浴磁力搅拌碱消解火焰原子吸收分光光度法测定土壤中铬（Ⅵ）。称取5.00 g土壤样品置于250mL聚乙烯瓶中，以20 g/L氢氧化钠和30 g/L碳酸钠碱性提取液提取，提取温度为93℃，提取时间为75 min；加入400mg氯化镁，调节滤液p H值为7.0～8.0。铬（Ⅵ）质量浓度在0.0～2.0 mg/L范围内线性相关系数为0.999 5，检出限为0.4 mg/kg。该方法应用于低、中、高3种铬（Ⅵ）土壤国家标准物质的分析，测定值与认定值相符，测定值的相对标准偏差为5.0%～7.7%(n=12)。     

反相高效液相色谱法测定土壤中氰溴甲苯

提出了反相高效液相色谱法同时测定土壤中氰溴甲苯的方法。样品采用索氏提取法,以二氯甲烷为提取溶剂提取6 h。提取液以ODS-C18色谱柱(150 mm×6 mm,5μm)为分离柱,以甲醇-水(70+30)为流动相经色谱分离,在检测波长为237 nm处进行测定。氰溴甲苯的质量浓度在0.6~10.0 mg.L-1范围内与其峰面积呈线性关系。标准加入回收率在85.0%~95.7%之间,相对标准偏差(n=6)在1.9%~10.3%之间。     

土壤与沉积物样品中多氯联苯总量的气相色谱-质谱法快速分析

建立了土壤和沉积物样品中多氯联苯总量的快速分析方法.样品经加速溶剂萃取,Bond ElutPCB SPE小柱净化后,采用气相色谱-质谱测定多氯联苯的总量,方法的平均回收率为84% ～106%,相对标准偏差为4.2% ～8.4%,多氯联苯总量的方法检出限为2.25 ng/g.该方法快速、灵敏、准确,适用于大部分土壤及沉积物样品中多氯联苯总量的快速筛查分析.     

加速溶剂萃取-凝胶色谱净化-气质联用测定土壤中15种有机氯农药残留的方法研究

建立了加速溶剂萃取-凝胶色谱净化-气质联用同时测定土壤中15种有机氯农药的分析方法。优化了凝胶色谱(GPC)净化的条件,比较了凝胶色谱净化及浓硫酸净化法对15种有机氯回收率的影响。结果表明,采用GPC净化能够有效避免浓硫酸净化对氯丹、异狄氏剂、硫丹、甲氧滴滴涕等农药回收率的影响,GPC净化的最佳收集时间为10~15 min,15种有机氯农药的回收率为56%~122%。15种有机氯农药在0.03~6.0 mg/L范围内具有较好的线性,相关系数达0.999以上,方法的检出限为0.1~5.0μg/kg,定量下限为0.4~16.0μg/kg。采用该方法对实际样品进行加标回收率实验,土壤样品的加标回收率为68%~122%,相对标准偏差为1.2%~5.9%。该方法简单、快捷、灵敏度高,已用于实际土壤样品的检测。     

Isolation and Characterization of Two Novel Gene Encoded Alkaline Esterases from an Alkaline Soil Metagenomic Library

<正>The development of industrial biotechnology has created an increasing demand for alkaline lipolytic enzymes with functional diversity.In this study,an alkaline soil metagenomic library was constructed to search for new lipolytic enzymes.Two novel gene encoded alkaline esterases(designated as estA and estB) were isolated by functional screening from the library.The estA gene consisted of 834 bp and coded for 277 amino acids with a molecular mass of 29998.Amino acid sequence homology analysis indicates that EstA belongs toα/βhydrolase fold family 4.4(abH4.4),with EstA being the smallest member of that family yet reported.The estB gene consisted of 1185 bp and encoded 394 amino acids with a theoretical molecular mass of 40090.Its conserved domain analysis shows that EstB belongs to the GDSL hydrolase superfamily.Both EstA and EstB exhibit only moderate identity(38%) in amino acid sequence to the known lipolytic enzyme genes in the database.The two genes were respectively expressed in Escherichia coli and the protein products were purified for functional characterization.While the expressed EstA did not exhibit the functional properties that were superior to those of other esterases previously reported,the EstB was stable at temperature up to 45℃and its maximum activity was measured to be 53.6 U/mg at pH=10.Both the enzymes have further enriched the diversity of the lipolytic enzymes database and also appear to be promising biocatalysts for potential biotechnological application.     

超高效液相色谱-串联质谱法研究阿维菌素在苹果和土壤中的残留消解动态

建立了苹果和土壤中阿维菌素残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法,并且应用本方法研究产自泰安、西安及北京的苹果和土壤中阿维菌素的代谢规律.样品经乙腈萃取后,用饱和NaCl盐析分层,静置30 min后,旋转蒸发浓缩,氨基柱净化,应用UPLC-MS/MS选择多反应监测(MRM)正离子模式扫描测定.本方法最低检出浓度(LOQ)为1.0 μg/kg(S/N=10);在2.0～100.0 μg/L范围内阿维菌素的峰强度与质量浓度的线性关系良好(r=0.9994).3个添加水平(1.0, 10和100 μg/kg)的平均回收率在79.2%～96.1%,相对标准偏差3.18%～9.14%.田间测定试验结果表明:阿维菌素在苹果中的原始沉积量为11.8～18.4 μg/kg,在土壤中的原始沉积量为44.7～54.8 μg/kg,代谢速率快,在苹果中的半衰期为2.35～3.84 d,在土壤中的半衰期为4.58～6.45 d.