西洋参根中微量元素

经对美国产与国产西洋参根中24种微量元素的测定,其中为生命活动所必需的元素有16种,如Fe、Cu、Zn、Mn、Mo、Cr、Co、Se、Ni、I、B、Ti等;具有明显抗癌活性和保护心血管系统的元素含量,国产洋参除Mn稍低外,其他元素Mo、mg、B、Ca、Se、Zn等均高于美国洋参。     

ICP-MS法测定狼毒中12种元素

目的建立电感耦合等离子质谱(ICP-MS)法测定狼毒药材中铝、铁、锰、锌、钡、镍、硒、铅、砷、汞、镉和铜等12种微量元素的方法。方法样品微波消解后,采用电感耦合等离子质谱仪测定了12种微量元素的含量,并进行了方法学研究。结果 12种元素校正曲线线性关系良好,回收率符合痕量分析要求。结论所建立的方法准确、可靠,为狼毒药材的研究提供了依据。     

加味四妙丸有效部位群HPLC指纹图谱归属分析及谱效关系研究

目的:明确加味四妙丸有效部位群中指纹图谱共有峰与组方药材有效部位及药效的相关性,表征加味四妙丸有效部位群药效物质基础。方法:用指纹图谱共有峰相对保留时间的相对偏差△t和紫外光谱夹角余弦特征相似度,考察共有峰与药材有效部位的相关性;将加味四妙丸中各有效部位及各组方药中的有效部位进行正交组合,测定指纹图谱及评价抗炎、镇痛及降尿酸作用,运用数理统计学的方法将药理数据与指纹图谱各色谱峰相对面积相关联,研究谱效相关性。结果:该方有效部位群12个共有峰分别来源于组方药苍术皂苷、黄柏皂苷、黄柏生物碱、土茯苓皂苷部位,与抗炎、镇痛、降尿酸作用均有相关性。结论:研究有效部位群指纹图谱共有峰的成分特征及谱效关系,是表征复方整体成分-配伍-药效相关性的有效途径。     

基于ICP-MS对不同产地小根蒜无机元素的主成分分析和聚类分析

目的:研究小根蒜中无机元素的含量及其分布特征,为中药材薤白的品质评价和质量控制提供实验依据。方法:采用电感耦合等离子体质谱(ICP-MS)法,对10个小根蒜样品中14个无机元素的含量进行全定量分析,从元素组学的角度建立其无机元素特征谱,并采用SPSS聚类分析和主成分分析对其特征元素进行评价。结果:主成分分析选出6个主因子,得出小根蒜的特征元素为Cu、Zn、Fe、Mn、Ni、Cr、Se;聚类分析将10个小根蒜样品聚为2大类,不同产地小根蒜体内无机元素的含量与气温、地理位置等生态环境存在着一定的相关性。结论:全定量分析法可用于小根蒜无机元素的含量测定;主成分分析法和聚类分析法是小根蒜无机元素含量分析的有效方法。     

ICP-AES法同时测定碳酸锂原料药中6种杂质元素

目的：建立电感耦合等离子体发射光谱（ICP-AES)同时测定碳酸锂原料药中6种杂质元素（钙、钠、钾、镁、铁和铝）的分析方法,并分析不同厂商碳酸锂原料药的杂质含量。方法：用硝酸溶解样品, ICP-AES法分析样品中6种杂质元素的含量。结果：6种元素标准曲线的相关系数均高于0.999,加标回收率为93%～99%,检出限为0.0003～0.1275μg·mL-1,RSD值均小于2%;利用本法对5个厂家使用的碳酸锂原料药进行测定,结果表明C厂的原料药中钙、钠、镁、铁和铝元素含量均高于其余4个厂家,其中钠超出了药典规定限度。结论：与《中国药典》中碳酸锂原料药杂质测定方法进行比对,本试验所建立的方法测定结果与药典方法一致,且方法专属性强、灵敏度高、操作简单,可以用于碳酸锂原料药中6种杂质元素的测定。     

Recent advances in trace analysis of pharmaceutical genotoxic impurities

Genotoxic impurities (GTIs) in pharmaceuticals at trace levels are of increasing concerns to both pharmaceutical industries and regulatory agencies due to their potentials for human carcinogenesis. Determination of these impurities at ppm levels requires highly sensitive analytical methodologies, which poses tremendous challenges on analytical communities in pharmaceutical R&D. Practical guidance with respect to the analytical determination of diverse classes of GTIs is currently lacking in the literature. This article provides an industrial perspective with regard to the analysis of various structural classes of GTIs that are commonly encountered during chemical development. The recent literatures will be reviewed, and several practical approaches for enhancing analyte detectability developed in recent years will be highlighted. As such, this article is organized into the following main sections: (1) trace analysis toolbox including sample introduction, separation, and detection techniques, as well as several ‘general’ approaches for enhancing detectability; (2) method development: chemical structure and property-based approaches; (3) method validation considerations; and (4) testing and control strategies in process chemistry. The general approaches for enhancing detection sensitivity to be discussed include chemical derivatization, ‘matrix deactivation’, and ‘coordination ion spray-mass spectrometry’. Leveraging the use of these general approaches in method development greatly facilitates the analysis of poorly detectable or unstable/reactive GTIs. It is the authors’ intent to provide a contemporary perspective on method development and validation that can guide analytical scientists in the pharmaceutical industries.     

孕期重金属元素和微量元素水平与子代先天性心脏病相关性的前瞻性队列研究北大核心CSCD

目的探讨孕期重金属元素和微量元素水平与子代先天性心脏病(简称先心病)的相关性,并建立孕期重金属元素和微量元素水平与子代先心病发生概率的预测模型。方法基于2010~2012年在甘肃省妇幼保健院开展的前瞻性出生队列研究,采用巢式病例对照研究方法,对14359名孕妇进行随访观察,以随访观察期内其子代确诊先心病的97名孕妇为先心病组,从队列人群中以1∶2的比例匹配194名子代未患先心病的孕妇为对照组。采用电感耦合等离子体质谱测定孕母孕20~24周时血液样本和胎儿脐血样本中的重金属元素和微量元素水平。采用多因素logistic回归分析评估重金属元素和微量元素水平与子代先心病之间的关联,并构建孕期重金属元素和微量元素水平与子代先心病发生概率的列线图预测模型。结果与对照组相比,先心病组孕妇血液样本中铝(aluminium,Al)、钠(natrium,Na)、钙(calcium,Ca)、钛(titanium,Ti)、硒(selenium,Se)、锶(strontium,Sr)、锡(stannum,Sn)、锑(stibium,Sb)、钡(barium,Ba)、钍(thorium,Th)水平较高,差异有统计学意义(P<0.05);先心病组脐血样本中Al、锌(zinc,Zn)、镁(magnesium,Mg)、钾(kalium,K)、Ca、Ti、铬(chromium,Cr)、铜(copper,Cu)、砷(arsenic,As)、Se、Sr、银(argentum,Ag)、镉(cadmium,Cd)、Sn、铅(plumbum,Pb)水平显著高于对照组(P<0.05)。多因素logistic回归分析显示,孕妇血液样本中Sb水平升高,其子代患先心病的风险显著增加(^(a)OR=4.81,P=0.004);而在脐血样本中,高浓度水平的Al(^(a)OR=4.22,P=0.013)、Mg(^(a)OR=8.00,P=0.014)、Pb(^(a)OR=3.82,P=0.049)与先心病的发生风险增加存在关联。孕期重金属元素和微量元素水平与子代先心病的预测模型中纳入的变量有:孕妇血Al、Th、Sb水平和脐血Al、Mg、Pb水平,绘制的列线图预测模型的校正曲线趋近于理想曲线。结论孕期Al、Th、Sb、Mg、Pb水平升高提示子代罹患先心病的风险增加,联合以上指标构建的列线图预测模型可以预测子代先心病的发生概率。     

Recovery and Separation of Dysprosium from Waste Neodymium Magnets through Cyphos IL 104 Extraction

In the present study, the extraction of rare earth elements (REEs) from waste neodymium magnets using phosphorus ionic liquid Cyphos IL 104 was investigated. The objective was to recover and separate the heavy REE (Dy) from light REEs (Nd and Pr). Therefore, the experimental parameters of ionic liquid extraction, including contacting time, the initial pH value, extractant concentration, and O/A ratio, have been optimized. The highest separation factor α_Dy/Nd of 45.18 and α_Dy/Pr of 47.93 has been achieved. Following the ionic liquid extraction, the comparison of different stripping agents and the stripping parameters (the concentration of stripping agent and A/O ratio) were also explored. In short terms, this research demonstrates the optimal parameters of Cyphos IL 104 for selectively extracting high REE (Dy) and reveals its potential for recovering and separating REEs in real waste.     

Trace Element Contents in Petrol-Contaminated Soil Following the Application of Compost and Mineral Materials

The global use of petroleum hydrocarbons as raw materials and an energy source in industry results in serious environmental, health, and ecological problems. Consequently, there is growing interest in the development of technologies for the rehabilitation of contaminated areas. This study was undertaken in order to determine the effect of different phytostabilising materials (compost, bentonite, and CaO) on the trace element content in soil contaminated with unleaded petroleum 95 (0, 2.5, 5, and 10 cm³ kg⁻¹ of soil). The doses of petroleum applied to the soil were based on the previously conducted preliminary experiment. The highest petroleum dose (10 cm³ kg⁻¹ of soil) significantly reduced the chromium, zinc, and cobalt contents in the soil. Petroleum increased the cadmium, lead, nickel, and copper contents in the soil. The materials used for phytostabilisation (compost, bentonite, calcium oxide) had a significant effect on the trace element content in the soil. The application of mineral materials (bentonite and calcium oxide) was more effective than the application of compost, compared to the control series (without soil amendments) as they reduced the contents of cadmium, chromium, nickel, and cobalt in the soil to the greatest extent. The reduction effect of bentonite and calcium oxide on the content of these trace elements in the soil was stronger than compost.     

Association of Gut Microbiota Enterotypes with Blood Trace Elements in Women with Infertility

Infertility is defined as failure to achieve pregnancy within 12 months of unprotected intercourse in women. Trace elements, a kind of micronutrient that is very important to female reproductive function, are affected by intestinal absorption, which is regulated by gut microbiota. Enterotype is the classification of an intestinal microbiome based on its characteristics. Whether or not Prevotella-enterotype and Bacteroides-enterotype are associated with blood trace elements among infertile women remains unclear. The study aimed to explore the relationship between five main whole blood trace elements and these two enterotypes in women with infertility. This retrospective cross-sectional study recruited 651 Chinese women. Whole blood copper, zinc, calcium, magnesium, and iron levels were measured. Quantitative real-time PCR was performed on all fecal samples. Patients were categorized according to whole blood trace elements (low levels group, <5th percentile; normal levels group, 5th‒95th percentile; high levels group, >95th percentile). There were no significant differences in trace elements between the two enterotypes within the control population, while in infertile participants, copper (P = 0.033), zinc (P < 0.001), magnesium (P < 0.001), and iron (P < 0.001) in Prevotella-enterotype was significantly lower than in Bacteroides-enterotype. The Chi-square test showed that only the iron group had a significant difference in the two enterotypes (P = 0.001). Among infertile patients, Prevotella-enterotype (Log(P/B) > −0.27) predicted the low levels of whole blood iron in the obesity population (AUC = 0.894; P = 0.042). For the high levels of iron, Bacteroides-enterotype (Log(P/B) <−2.76) had a predictive power in the lean/normal group (AUC = 0.648; P = 0.041) and Log(P/B) <−3.99 in the overweight group (AUC = 0.863; P = 0.013). We can infer that these two enterotypes may have an effect on the iron metabolism in patients with infertility, highlighting the importance of further research into the interaction between enterotypes and trace elements in reproductive function.