目的建立微波消解-电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry,ICP-MS)测定面制食品中Al元素含量的方法。方法面制食品样品经微波消解后,使用ICP-MS测定,并对方法的线性范围、检出限、精密度和回收率等进行...目的建立微波消解-电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry,ICP-MS)测定面制食品中Al元素含量的方法。方法面制食品样品经微波消解后,使用ICP-MS测定,并对方法的线性范围、检出限、精密度和回收率等进行考察。结果 Al元素在20.0~200.0μg/kg范围内的相关系数大于0.999,线性良好,方法检出限为0.2μg/kg,定量限为0.6μg/kg。加标浓度为5.0~15.0μg/kg时,回收率在99.3%~105.0%之间,且相对标准偏差(relative standard deviation,RSD)在0.93%~2.11%之间。结论该检测方法简单、快速、准确、灵敏度高,适用于面制食品中Al元素的测定。展开更多
目的建立电感耦合等离子体质谱法测定大米中16种稀土元素含量。方法称取0.2 g左右的大米,加入7mL硝酸,在120℃下进行预消解,预消解完成后进行微波消解,定容摇匀待测。在已优化过的电感耦合等离子体质谱仪上测定大米中16种稀土元素,并对...目的建立电感耦合等离子体质谱法测定大米中16种稀土元素含量。方法称取0.2 g左右的大米,加入7mL硝酸,在120℃下进行预消解,预消解完成后进行微波消解,定容摇匀待测。在已优化过的电感耦合等离子体质谱仪上测定大米中16种稀土元素,并对其线性回归方程、检出限、精密度和回收率等进行考察。结果16种稀土元素在一定范围内线性关系良好,相关系数均大于0.995,方法检出限为0.002~0.440μg/kg,定量限为0.006~1.480μg/kg。各元素加标回收率在85.7%~107.9%,测定结果相对标准偏差(relative standard deviation,RSD)在1.8%~4.5%。结论该检测方法简单、快速、选择性好、灵敏度和回收率高,适用于大米中多种稀土元素的测定。展开更多
Five PAHs haptens 3 a～3 e were synthesized from naphthalene, anthracene, chrysene, pyrene and acenaphthene via two steps including Friedel-Crafts acylation and WolffKishner-Huang reduction. The sixth hapten 4-(acenap...Five PAHs haptens 3 a～3 e were synthesized from naphthalene, anthracene, chrysene, pyrene and acenaphthene via two steps including Friedel-Crafts acylation and WolffKishner-Huang reduction. The sixth hapten 4-(acenaphthylen-3-yl)butanoic acid(3 f) was prepared from hapten 3 e via three steps including esterification, bromination and elimination. Their structures were confirmed by melting point, ~1H NMR and ^(13)C NMR. Their optical properties and crystal structures were also investigated. The results of density functional theory(DFT) calculation provided the supports that the size, shape(geometry) and electronic properties at the corresponding parts of 3 a～3 f did not change significantly, compared to those of PAHs. The haptens 3 a～3 f were coupled with bovine serum albumin(BSA) to make antigens. The coupling ratios were 1:20～1:38. These results show that the haptens could be used to induce specific antibodies for PAHs.展开更多
文摘目的建立微波消解-电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry,ICP-MS)测定面制食品中Al元素含量的方法。方法面制食品样品经微波消解后,使用ICP-MS测定,并对方法的线性范围、检出限、精密度和回收率等进行考察。结果 Al元素在20.0~200.0μg/kg范围内的相关系数大于0.999,线性良好,方法检出限为0.2μg/kg,定量限为0.6μg/kg。加标浓度为5.0~15.0μg/kg时,回收率在99.3%~105.0%之间,且相对标准偏差(relative standard deviation,RSD)在0.93%~2.11%之间。结论该检测方法简单、快速、准确、灵敏度高,适用于面制食品中Al元素的测定。
文摘目的建立电感耦合等离子体质谱法测定大米中16种稀土元素含量。方法称取0.2 g左右的大米,加入7mL硝酸,在120℃下进行预消解,预消解完成后进行微波消解,定容摇匀待测。在已优化过的电感耦合等离子体质谱仪上测定大米中16种稀土元素,并对其线性回归方程、检出限、精密度和回收率等进行考察。结果16种稀土元素在一定范围内线性关系良好,相关系数均大于0.995,方法检出限为0.002~0.440μg/kg,定量限为0.006~1.480μg/kg。各元素加标回收率在85.7%~107.9%,测定结果相对标准偏差(relative standard deviation,RSD)在1.8%~4.5%。结论该检测方法简单、快速、选择性好、灵敏度和回收率高,适用于大米中多种稀土元素的测定。
基金supported by the Natural Science Foundation of Jiangsu Province(BK20161542)the Natural Science Foundation of the Higher Education Institutions of Jiangsu Province(16KJB550005 and 17KJB150006)+1 种基金Jiangsu Overseas Visiting Scholar Program for University Prominent Young&Middle-aged Teachers and Presidents(2017)the Youth Foundation of Southeast University Chengxian College(y0004)
文摘Five PAHs haptens 3 a～3 e were synthesized from naphthalene, anthracene, chrysene, pyrene and acenaphthene via two steps including Friedel-Crafts acylation and WolffKishner-Huang reduction. The sixth hapten 4-(acenaphthylen-3-yl)butanoic acid(3 f) was prepared from hapten 3 e via three steps including esterification, bromination and elimination. Their structures were confirmed by melting point, ~1H NMR and ^(13)C NMR. Their optical properties and crystal structures were also investigated. The results of density functional theory(DFT) calculation provided the supports that the size, shape(geometry) and electronic properties at the corresponding parts of 3 a～3 f did not change significantly, compared to those of PAHs. The haptens 3 a～3 f were coupled with bovine serum albumin(BSA) to make antigens. The coupling ratios were 1:20～1:38. These results show that the haptens could be used to induce specific antibodies for PAHs.
