UHPLC-Q/TOF MS结合HPLC-DAD定性和定量分析硫酸黏菌素可溶性粉中的未知添加物

定性和定量分析一批兽药硫酸黏菌素可溶性粉中的未知添加物。照《中国兽药典》2010年版一部对该批检品用微生物检定法进行含量测定时,发现该样品的抑菌圈为虚圈,用薄层色谱鉴别该样品,未显示与标准品溶液一致的主斑点,怀疑该样品中有处方外非法添加物。采用超高效液相色谱-四级杆-飞行时间质谱(UHPLC-Q/TOF MS)对该样品进行筛查,发现疑似添加物,并使用液相色谱-二极管阵列检测(HPLC-DAD)法进行了双重确证和含量测定。该样品中非法添加物确证为磺胺氯达嗪和甲氧苄啶,添加量分别为58.5 mg/g和13.4 mg/g。本研究通过建立筛查方法为监管部门提供技术支撑,通过分析非法添加物的可能原因为打击兽药处方外非法添加提供了思路。     

Intra‐abdominal cystic lymphangiomatosis in a Thoroughbred foal

Cystic lymphangiomas are rare malformations of the lymphatics that result in the formation of a cystic mass. Where multiple cysts are seen, the condition is termed cystic lymphangiomatosis. This case describes the diagnosis and unique management of cystic lymphangiomatosis in a 10‐day‐old Thoroughbred foal. Ultrasonography, histopathology and laparoscopy were essential for diagnosis and appreciation of the extent of disease. Ultimately, the cystic lymphangiomatosis was so extensive in this foal that complete surgical excision was considered impossible and the presence of adhesions within the abdomen indicated a very poor long‐term prognosis; the owners elected for euthanasia at age 14 weeks. Although rare, lymphangioma and lymphangiomatosis should be considered as a differential diagnosis for an intra‐abdominal mass in a young horse.     

水利施工的大体积混凝土抗裂技术

混凝土是水利施工中的主要的应用材料之一，为了保证水利施工中的安全与质量，必须保证混凝土的质量。文章全面分析了大体积混凝土产生裂缝的原因，并给出了相应的控制方法。     

Perivascular wall tumour presenting as pastern mass in a Standardbred gelding

A 2-year-old Standardbred gelding was referred for a mass on the palmaromedial right front pastern which was accompanied by progressively worsening lameness. The mass was firm to palpation and covered by normal skin. Ultrasonographically, a smooth encapsulated mass was present, medial to the flexor tendons and palmar to the neurovascular bundle. Because of a poor prognosis for future athletic performance without surgical or chemotherapeutic intervention and economic constraints preventing further diagnostics and treatment, the horse was euthanised. Post-mortem magnetic resonance imaging, histopathology and immunohistochemistry revealed the mass to be a perivascular wall tumour, the first record of such a neoplasia in the horse.     

半胱胺对育成期水貂生长和饲料转化率的影响

选择健康育成期水貂208只,其中200只为试验组,8只为对照组,采用二因子试验设计:一个因子为半胱胺的不同添加量,分别按每千克体质量添加10、40、70、100、130 mg半胱胺;另一因子为半胱胺的不同添加间隔时间,分别为1、3、5、7、9 d 5个时间间隔.通过饲养试验研究了半胱胺对育成期水貂体质量增加、饲料转化率...     

磷酸、膦酸酯类农药的质谱裂解规律研究

在对23种磷酸、膦酸酯类农药及其氧化物的质谱数据进行归纳整理的基础上,明确了这类农药质谱裂解规律。结果表明:电子轰击离子化条件下,磷酸、膦酸酯类农药分子极易裂解,且分子离子峰较弱。发现C_2H_6O_3P~+(m/z109)是其最具代表性的特征碎片离子。磷酸酯类农药裂解规律是二甲氧基磷酸酯P-0键易发生a断裂,生成m/z 109特征碎片离子。二乙氧基磷酸酯易脱去中性碎片C_2H_4,形成m/z81的特征离子。R'含有烯烃结构,易产生m/z127的特征碎片离子。膦酸酯类农药裂解规律与磷酸酯类似,特征性弱,膦键容易发生a断裂。选定了磷酸、膦酸酯类农药在质谱分析中常见的碎片离子,为农药残留筛查、确证分析提供参考。     

Computed Tomography and Magnetic Resonance Imaging of an Epidermoid Cyst in a Foot of a Horse

An 18-year-old Quarter Horse mare was evaluated because of moderate left forelimb lameness of 4 weeks’ duration. The clinical evaluation and diagnostic perineural analgesia localized the lameness to the distal portion of the left forelimb. There was swelling on the dorsal and lateral aspect of the coronary band. Radiography, ultrasound, magnetic resonance imaging, and computed tomography of the foot revealed circumscribed well-capsulated soft tissue mass causing a focal deformation of the dorsolateral border of the middle phalanx. The treatment aimed to remove the mass surgically and stabilized the interphalangeal joint, but the owner elected human euthanasia before treatment attempt. Histopathology diagnosis was an epidermoid cyst, which was characterized by multilayers of keratin surrounded by stratified squamous epithelium. Although rare, an epidermoid cyst should be considered as a differential diagnosis for space-occupying mass in horses’ foot that develops chronic lameness after trauma. This report describes the multimodality appearance of the epidermoid cyst.     

A systematic approach to determine the impact of elevated CO2 levels on the chemical composition of wheat (Triticum aestivum)

Two wheat genetic lines (responsive and non-responsive to elevated CO₂) grown under ambient and free-air CO₂ enrichment (FACE) conditions were compared using fuzzy chromatography mass spectrometry (FCMS) metabolite fingerprinting. A more comprehensive survey of the changes in their chemical composition was made on selected samples using ultra-high-performance liquid chromatography (UHPLC) metabolomic profiling with high resolution accurate mass/tandem mass spectrometry (HRAM/MSⁿ). Principal component analysis (PCA) of the metabolite fingerprints showed four clusters for the two genetic lines (responsive and non-responsive) and the two CO₂ levels (ambient and elevated) in score plots. Metabolite profiling of representative samples for each of the four clusters identified 25 and 16 compounds from negative and positive data, respectively, including amino acids, saccharides, phenolic acids, flavonoids, and lipids. Loading plots demonstrated that some saccharides and lipids were responsible for discriminating between not only two genetic lines but also two CO₂ levels. Analysis of free amino acids (not bound) showed a clear pattern of reduced concentration for both lines with elevated CO₂. After acid hydrolysis, the responsive line 6 (41% increase in yield) showed the same pattern observed for free amino acids, but the non-responsive line 5 (6% increase in yield) showed different trends in concentrations of amino acids with elevated CO₂.     

超高效液相色谱串联质谱法对水产品中硝基呋喃代谢物的测定

建立了使用Waters UPLC Xevo TQ超高效液相色谱串联质谱仪检测水产品中4种硝基呋喃代谢物的分析方法。匀浆后的样品在酸性环境下水解,并用2-硝基苯甲醛衍生16h,经磷酸氢二钾提取,LMS固相萃取小柱净化后,在三重四极杆多反应监测模式下进行测定。方法采用同位素内标法定量,四种代谢物的检出限(LOD)均低于0.25μg·kg-1,线性范围在0.5μg·L~(-1)到10μg·L~(-1)间,相关系数大于0.99。在0.5、1.0和5μg·kg-1浓度下分别进行添加回收试验(n=5),回收率在75.2%~123.3%之间,相对标准偏差(RSD)小于9.4%。