泰和乌骨鸡肉模拟胃肠道消化液中ACE抑制肽的分离纯化及结构鉴定

研究泰和乌骨鸡肉在胃肠道消化过程中的降血压活性,并鉴定出其中确定具有降血压活性的肽序列。采用体外模拟胃肠道消化法,测定了不同阶段消化液对血管紧张素I转化酶(ACE)的抑制作用,并选择其中的小肠道消化液,对其进行超滤、制备型反相高效液相色谱、凝胶柱色谱分离纯化,最后通     

微波消解-ICP-MS测定动物血清和组织器官中的微量银元素

银的应用在当代生物医学领域得到极大地推广,其生物安全性也受到密切关注,明确银离子在生物体内分布以及其安全阈值显得格外重要。因此,需要一种高灵敏度的分析方法来确定医学生物样品中银的含量。电感耦合等离子体质谱(ICP-MS)法对于金属离子检测具有很高的灵敏度,非常适用于医学生物样品中所含痕量银元素的检测,但具体方法的开发,包括样品前处理和检测过程,尚处于起步阶段。本研究建立了一套简便易行的微波消解处理机体血清和组织器官样品,通过ICP-MS法测定样品内微量银元素的检测方法。血清和肌肉、骨髓、骨骼组织,以及心脏、肝脏、脾脏、肾脏器官样品经5 mL硝酸-2 mL过氧化氢体系微波消解。消解程序采用2 000 W功率3步式温度梯度,样品最终消解完全,获得的数据重复性好,且耗费时间短,为大批量样品处理节省了时间。消解溶液经稀释定容,在优化仪器工作参数后,用ICP-MS对溶液中的107Ag进行测定,以钇(Y)为内标元素补偿基体效应和准确度漂移。测定结果显示,107Ag元素检出限为0.98 μg·kg-1,标准曲线相关系数为0.999 9,回收率为98%～107%,相对标准偏差(RSD)为2.0%～4.3%。用该法测定了动物血清和组织器官中的银元素含量,发现机体摄入银离子后,主要蓄积在肝脏。检测结果表明ICP-MS方法可以准确地测定机体的微量银元素,所建立的方法适用性强,可满足不同类型医学生物样品中微量银元素的测定,操作简便快捷,结果准确且灵敏度高,尤其适合于大批量生物样品的检测,为其他生物样品微量元素的检测提供了指导。     

微波消解ICP-MS测定铝塑包装材料中的Pb,Cr,Cd和As含量

通过微波消解法对铝塑包装材料的前处理方法进行了深入的研究,考虑了5种不同的消解试剂组合以及不同的浓度配比关系对铝塑包装材料消解效果的影响,并对消解现象产生的可能性原因进行了简单的分析,结果发现硫酸-硝酸试剂组合消解效果最佳,正交试验结果表明试剂组合的最佳配比为1∶7.随后采用电感耦合等离子体质谱法(ICP-MS)测定了铝塑包装材料中的Pb,Cr,Cd和As,各元素仪器检出限依次为0.215,0.067,0.006和0.020 ng·mL-1,线性相关系数在0.999 5以上;2#试样进行加标回收试验,回收率在83.8%~111.6%之间,相对标准偏差(RSD)在0.5%~7.4%之间;5种试样两次独立平行测定结果均比较接近,t检验法(取置信水平α=0.05)结果表明两次测定结果均无显著性差异.综上表明该方法线性关系好,检出限低,回收率高,精密度好,可准确测定铝塑包装材料及类似材料中的Pb,Cr,Cd,As含量.     

微波消解ICP-AES法分析九种补血类中药元素

采用微波消解法处理样品,以电感耦合等离子体发射光谱法(ICP-AES)测定并分析九种补血类中药中Zn,Mn,Na,K,Ca,Mg,Ni,Pb,Se,Fe,Cu,Al,B,Ti,Sn,Hg和Li元素的含量。结果显示,九种补血类中药富含有益于人体健康的主要及微量元素,其中众所周知补血类元素Fe,Se,Ni,Mn,Zn含量较高。九种补血中药按各大元素分类(大量元素,必需元素,非必需元素,有害元素)分布于柱形直方图。应用主成分分析和聚类分析于数据矩阵去评价元素分析结果。聚类分析的结果显示九种补血类中药中十七种元素的含量所形成的树状系统图主要分为三个集群。通过优化微波消解条件,各元素的回收率均在97.89%～103.25%之间,相对标准偏差均小于3.0%。ICP-AES结合微波消解法可以精确和准确地测定九种补血类中药中的元素。     

不同消解方式对土壤中锑的原子荧光法检测影响

氢化物发生-原子荧光光谱法是土壤环境中锑检测所广泛使用的方法．土壤的消解前处理分别采用王水微波消解（半消解）、混酸全消解（硝酸＋高氯酸＋氢氟酸）方式．研究结果表明王水微波消解对锑的检测效果较好,标准土壤9次测定值的相对标准偏差为3．6％,实际样品的回收率为96％-102％．而采用混酸全消解的方式测定值偏低,实际样品的回收率为78％～86％,而且精密度超过5％,这是由于在赶酸过程中样品易被蒸干而造成痕量锑元素的损失．     

Chemical analysis of Gothic mortar from a bridge pier in Roudnice nad Labem (Czech Republic)

In this paper, a Gothic mortar originating from the remains of a bridge pier in Roudnice nad Labem (Czech Republic) was analyzed. The inorganic composition of the mortar showing special mechanical properties was studied using polarizing light microscopy, scanning electron microscopy coupled with energy dispersive X-ray spectrometry, and X-ray diffraction, while the protein content was analyzed by peptide mass mapping using matrix-assisted laser desorption/ionization—time of flight mass spectrometry and nanoliquid chromatography coupled to tandem mass spectrometry. Two types of inorganic binders having a composition similar to mineral wollastonite and hydraulic lime and milk protein additive were detected. We believe that organic and inorganic binders added together to the mortar increase its hardness and firmness in the aquatic environment.     

Effect of acid concentration on closed-vessel microwave-assisted digestion of plant materials

The efficiency of microwave-assisted acid digestion of plants using different concentrations of nitric acid (2.0, 3.0, 5.0, 7.0 and 14 mol l⁻¹) with hydrogen peroxide (30% v/v) was evaluated by measuring the residual carbon content (RCC) using inductively coupled plasma optical emission spectrometry (ICP-OES) with axial viewing. Certified reference materials were used for evaluating the accuracy attained when 2 mol l⁻¹ HNO₃ was employed for digestion. Under all experimental conditions RCC values were always lower than 13% w/v, and even the highest concentration did not cause any interference with element recovery. It seems that the high pressure reached for closed-vessel operation improved the oxidative action of nitric acid due to consequent temperature increase, even when this reagent was not used at high concentrations. According to acid–base titration data, residual acid in the digestates varied from 1.2 to 4.0 mol l⁻¹, depending on the acid concentration initially added. It can be concluded that for plant materials, microwave-assisted acid digestion can be carried out under mild conditions, which implies that digestates do not need extensive dilution before introduction by pneumatic nebulization to ICP-OES. An additional advantage is the lower amount of residue generated when working with less concentrated acid solutions.     

Determination of musk fragrances in sewage sludge by pressurized liquid extraction coupled to automated ionic liquid‐based headspace single‐drop microextraction followed by GC‐MS/MS

A method for the quantitative determination of ten musk fragrances extensively used in personal care products from sewage sludge was developed by using a pressurized liquid extraction (PLE) followed by an automated ionic liquid‐based headspace single‐drop microextraction and gas chromatography‐tandem mass spectrometry. The influence of main factors on the efficiency of PLE was studied. For all musks, the highest recovery values were achieved using 1 g of pretreated sewage sludge, H₂O/methanol (1:1) as an extraction solvent, a temperature of 80°C, a pressure of 1500 psi, an extraction time of 5 min, 2 cycles, a 100% flush volume, a purge time of 120 s, and 1 g Florisil as in‐cell clean‐up extraction sorbent. The use and optimization of an in‐cell clean‐up sorbent was necessary to remove fatty interferents of the PLE extract that make the subsequent ionic liquid‐based headspace single‐drop microextraction difficult. Validation parameters, namely LODs and LOQs, ranged from 0.5–1.5 to 2.5–5 ng/g, respectively. Good levels of intra‐ and interday repeatabilities were obtained analyzing sewage sludge samples spiked at 10 ng/g (n = 3, RSDs < 10%). The method applicability was tested with sewage sludge from different wastewater treatment plants. The analysis revealed the presence of all the polycyclic musks studied at concentrations higher than the LOQs, ranging from 6 to 530 ng/g. However, the nitro musk concentrations were below the LOQs or, in the case of musk xylene, was not detected.     

微波消解-FAAS法测定大别山区三种中药中的微量元素

采用微波消解-火焰原子吸收光谱(FAAS)法对大别山区3种中药(何首乌、黄精和拐枣)中的微量元素进行测定。用微波消解仪处理样品,对消解条件及消解程序进行优化,在最佳微波消解条件下,结合FAAS法测定上述3种中药中Ca、Mg、Cu、Zn、Fe、Mn 6种元素的含量。结果表明,微波消解的最佳条件为:何首乌和拐枣采用HNO3-H2O2混酸体系,配比分别为5∶2和5∶3,固液比1∶20,最高功率(700W)时的保温时间分别为8min和6 min;黄精采用HNO3-HCl,混酸体系,配比5∶2,固液比1∶28,保温时间为8 min。所建立的定量分析方法回收率为95.63%～101.36%,相对标准偏差小于3.0%,线性相关系数大于0.999,方法检出限为0.18～2.20 ng/mL。3种中药中均含有丰富的微量元素,尤其是黄精中Fe、Ca和Mn的含量较高;何首乌中Mg、Zn和Fe含量相对较高;拐枣中Fe和Ca含量相对较高。研究结果可为上述3种中药中微量元素的含量与其药效的相关性提供科学依据。     

微波消解-火焰原子吸收法测定玫瑰枝叶的5种微量元素

用微波消解一火焰原子吸收光谱法测定了玫瑰枝条和叶片中5种微量元素元素（钙、铜、铁、锰、镁）的含量。结果表明,玫瑰枝条和叶片中含有较丰富的镁、钙、铁,铜、锰含量较低,该法灵敏度高、快速、准确,所测数据可为玫瑰枝叶的合理利用提供可靠依据。