QuEChERS-GC-MS/MS法同时测定刺梨中15种有机氯农药残留

建立刺梨中15种有机氯农药残留的气相色谱-三重四级杆串联质谱（GC-MS/MS）检测法。刺梨样品采用QuEChERS前处理，正己烷溶液进行提取，经乙二胺-N-丙基硅烷（PSA）和C18各50 mg固相分散净化，浓缩定容后用GC-MS/MS法在多反应监测（MRM）模式下进行测定，通过保留时间、特征离子及其相对丰度定性，外标法定量。15种有机氯农药在0.05～1.00 μg/mL质量浓度范围内呈良好的线性关系，相关系数R2均＞0.997。分别向刺梨样品中分别加入标准品25 μg/kg、50 μg/kg、100 μg/kg时，加标平均回收率在81.98%～105.55%之间，相对标准偏差（n=6）均＜10%，检出限（S/N=3）在0.001 2～0.021 2 mg/kg。该方法具有经济、快速、灵敏度高、重现性好等优势，适用于食品中多种农药残留的同时快速测定。     

超高效液相色谱-串联质谱法测定动物源食品中克霉唑的残留量

目的建立QuEChERS提取和净化、超高效液相色谱-串联质谱(ultraperformanceliquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定猪肉、牛肉、羊肉、鸡肉等畜禽肉和猪肝、猪肾、羊肝、鸡心等畜禽内脏中克霉唑残留的分析方法。方法样品经正己烷饱和的乙腈提取,提取液经乙腈饱和的正己烷液液分配除脂,并经含PSA和C18粉末的净化管进一步净化。采用0.1%甲酸和乙腈作为流动相进行梯度洗脱,多反应监测模式(multiplereactionmonitoring,MRM)测定,同位素内标法定量。结果本方法在7 min内完成分离分析,方法在0.2～20.0μg/L范围内线性关系良好,相关系数r为0.9999。在0.2、2.0和20μg/kg添加水平下的回收率为78.5%～111.9%,相对标准偏差小于11.1%,方法定量限为0.2μg/kg。结论该方法快速、准确、灵敏,适合动物源食品中克霉唑残留量的测定。     

Compilation of Modern Technologies To Map Genome-Wide Cytosine Modifications in DNA

Over the past few decades, various DNA modification detection methods have been developed; many of the high-resolution methods are based on bisulfite treatment, which leads to DNA degradation, to a degree. Thus, novel bisulfite-free approaches have been developed in recent years and shown to be useful for epigenome analysis in otherwise difficult-to-handle, but important, DNA samples, such as hmC-seal and hmC-CATCH. Herein, an overview of advances in the development of epigenome sequencing methods for these important DNA modifications is provided.     

冶金矿物和产品水分测定问题探讨

水分测定是冶金行业中矿产原料和产品分析的重要内容,主要包括交货水分、湿存水、化合水等测定类别。尽管水分测定方法本身相对简单,但其涉及到矿物原料、产品结算交割以及其他化学分析的校正计算,属于重要的基础性测定方法。各类矿物、产品几乎都有相应水分测定的国家标准、行业标准,部分还是从国外ISO标准体系中采标而来。文章系统介绍并比较各类矿物原料、产品中交货水分、明水、湿存水、化合水等类别的测定方法。由于ISO标准体系中湿存水含义和国内标准体系湿存水含义有较大差异,其测定操作和用途也有不同,使用空气平衡样品和密封原始样品将会得到数据差异较大的湿存水数据,两种湿存水含义需要明确区分。湿存水对化学称样量、灼减量、化合水的测定有影响,需要用湿存水进行水分校正,才能得到更精确的结果。     

催化共振光散射法测定空气中痕量甲醛的研究

吖啶橙分子聚集体微粒可在513nm波长处出现最大的共振光散射强度(RLS)。在稀硫酸介质中,甲醛能催化溴酸钾氧化吖啶橙的反应,促使其RLS强度减弱。在最佳实验条件下,甲醛质量浓度ρ在0.020～0.25μg/mL的范围内与△I值呈良好的线性关系,线性回归方程为△I=1113.99ρ+49.23,线性相关系数r为0.9986。本法与国标法进行对照,在置信度等于95%时,用Cochran检验,两种方法间不存在显著性差异,方法操作简单、灵敏度高,用于室内外空气中甲醛测定,结果满意。     

钼蓝分光光度法联合测定铁矿石中磷和二氧化硅

以往铁矿石中磷和二氧化硅含量的测定需要分别采用钼蓝分光光度法。在使用磷钼蓝分光光度法时,常会因钒、砷等的干扰使得磷测定结果不准确,需要将样品再处理后才能测定。实验采用石墨垫底铁坩埚,碳酸钠和硼酸混合熔剂高温熔融铁矿石,使铁矿石样品分解彻底,再分别采用铋磷钼蓝和硅钼蓝分光光度法测定磷和二氧化硅含量,从而实现了采用钼蓝分光光度法联合测定铁矿石中磷和二氧化硅。干扰试验表明,在高温熔融时,石墨可将钒(V)还原为钒(III),使样品中钒不干扰磷的测定;显色液中加入15mg硫代硫酸钠溶液可将砷(V)还原为砷(III),继而消除砷对磷测定的干扰。磷的质量浓度在0~3μg/mL范围内遵守比尔定律,校准曲线的线性相关系数为0.9999,表观摩尔吸光系数为2.242×10⁴ L·mol^-1·cm^-1;二氧化硅的质量浓度在0~5μg/mL范围内遵守比尔定律,校准曲线的线性相关系数为0.9995,表观摩尔吸光系数为9.342×10³ L·mol^-1·cm^-1。方法中磷和二氧化硅的检出限分别为0.0026μg/mL和0.0081μg/mL。按照实验方法测定6个铁矿石标准样品中磷和二氧化硅,磷测定结果的相对标准偏差(n=8)小于5%,相对误差小于2%;二氧化硅测定结果的相对标准偏差(n=8)小于2%,相对误差小于1.5%。按照实验方法测定5个铁矿石样品中磷和二氧化硅,磷测定结果的相对标准偏差(RSD,n=8)小于7%,二氧化硅测定结果的相对标准偏差(n=8)小于1%;磷和二氧化硅的测定值均与电感耦合等离子体原子发射光谱法的测定值相一致。     

Determining Stability Constants Using the AKUFVE Technique

ABSTRACT

The AKUFVE techniques were developed by Rydberg and co-workers in the 1960s. The main aim was to be able to perform a series of liquid-liquid extraction data varying one or more parameters and at the same time achieve very pure phases. As such, this technique was later used for short-lived isotope studies in the SISAK system, but also as a standalone unit for a large number of thermodynamic studies of extraction systems both for fundamental understanding as well as more applied investigations. In this paper, the apparatus with modifications made over the decades is described. In addition, studies with stability constant determinations for the zirconium-water-acetylacetone system as well as lanthanide extraction using bromodecanoic acid are exemplified to demonstrate the potential use of the technique. The results shown clearly demonstrate the versatility and ability of the AKUFVE system.