Identification of Arcanobacterium pluranimalium by matrix-assisted laser desorption ionization-time of flight mass spectrometry and,as novel target,by sequencing pluranimaliumlysin encoding gene pla

In the present study 13 Arcanobacterium pluranimalium strains isolated from various animal origin could successfully be identified phenotypically by matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) and genotypically by sequencing 16S rDNA and the pluranimaliumlysin encoding gene pla. The detection of mass spectra by MALDI-TOF MS and the novel genotypic approach using gene pla might help to identify A. pluranimalium in future and might elucidate the role this species plays in infections of animals.     

Investigation of the Role of Androstenedione-19-oic Acid in the Presence of 19-Norandrostenedione in Intact Male Horse Plasma Using Liquid Chromatography–Tandem Mass Spectrometry

A liquid chromatography–tandem mass spectrometry method was developed to confirm the presence of androstenedione-19-oic acid in intact male equine plasma and to show the source of 19-norandrostenedione in equine plasma. Androstenedione-19-oic acid was recovered from acidified plasma by liquid–liquid extraction using methyl tert-butyl ether and separated on an Ace 5 C₈ column. A triple quadrupole mass spectrometer was used to detect the analytes in negative electrospray ionization mode. Limits of detection, quantification, and confirmation of the method were 0.1, 0.5, and 1.0 ng/mL, respectively. The linear dynamic range of quantification was 0.5–50 ng/mL. The presence of androstenedione-19-oic acid was confirmed in all plasma samples obtained from intact male horses but not those from gelded and female horses; the average concentration was 3.1 ± 1.6 ng/mL, suggesting androstenedione-19-oic acid is an endogenous compound only in intact male horse plasma samples. The conversion of androstenedione-19-oic acid to 19-norandrostenedione in equine plasma was demonstrated by spiking androstenedione-19-oic acid into blank plasma and monitoring the generation of 19-norandrostenedione and its increase in concentration during storage. Results indicated that androstenedione-19-oic acid was readily converted into 19-norandrostenedione; the higher the storage temperature, the faster the conversion. The conversion was not affected by the types of plasma samples collected from gelded and female horses or by anticoagulants used in blood collection to harvest plasma. Compared with other matrices such as water, methanol, and phosphate-buffered saline, the conversion of androstenedione-19-oic to 19-norandrostenedione in equine plasma was faster, suggesting that there is an unknown factor(s) in equine plasma that enhances the conversion.     

鸡肉和鸡蛋中金刚烷胺与金刚乙胺残留检测UPLC-MS/MS法研究

建立了鸡肉和鸡蛋中金刚烷胺与金刚乙胺残留检测的超高效液相色谱-串联质谱方法（UPLC-MS／MS）。样品在酸性条件下乙腈提取后,用正己烷去除脂肪,高速离心去除蛋白质等杂质,上机测试。液相色谱条件：色谱柱为BEHC18（50×2．1mm,1．7μm）,流动相为0．1％甲酸乙腈溶液＋0．1％甲酸水溶液,流速0．3mL／min,柱温30cI二,进样量10μL。质谱条件：电喷雾离子源（ESI^＋）,多反应监测（MRM）方式进行采集。结果表明：金刚烷胺与金刚乙胺在2～100ng／mL浓度范围内均呈现良好的线性关系,相关系数（R。）分别为=0．9977和0．9988;鸡蛋和鸡肉中金刚烷胺与金刚乙胺残留检测方法检测限均为1ng／g,定量限均为2ng／g。从鸡肉组织在2、5和10ng／g三个添加浓度检测结果可以看出,金刚烷胺与金刚乙胺的平均回收率分别为79．6％～107．5％和78．4％～101．2％,批内和批间RSD均小于15％。从鸡蛋在2、5和10ng／g三个添加浓度检测结果可以看出,金刚烷胺与金刚乙胺的平均回收率分别为90．8％～111．1％和75．4％～87．4％,批内和批间RSD均小于15％。该方法具有简便快捷、灵敏度高、定性准确等特点。     

UPLC-MS/MS测定4种兽药制剂中非法添加阿托品的方法研究

建立了兽药中非法添加药物阿托品的超高效液相色谱-串联质谱（UPLC-MS/MS）的检测方法。样品经提取稀释,采用BEH C18柱为分离柱,外标法定量。结果表明,阿托品在0.5～10 ng/mL范围内线性关系良好,相关系数大于0.99。在4～6 mg/g(或mg/mL)添加浓度范围内阿托品的平均回收率97.4%～110.9%,批内变异系数均小于10％,检测限为0.2 mg/g(或mg/mL),定量限为0.5 mg/g(或mg/mL)。该方法简便、灵敏度高、重现性好,适用于兽药中非法添加阿托品的含量测定。     

中华绒螯蟹副性征的研究

在解剖、测量性成熟和未成熟中华绒螯蟹外部形态和性腺之基础上,试用“双百分率法”和“差异显著性检测法”对中华绒螯蟹的副性征进行了研究。结果表明,性成熟后的雌、雄中华绒螯蟹均具有较明显的副性征。     

Accurate Dereplication of Bioactive Secondary Metabolites from Marine-Derived Fungi by UHPLC-DAD-QTOFMS and a MS/HRMS Library

In drug discovery, reliable and fast dereplication of known compounds is essential for identification of novel bioactive compounds. Here, we show an integrated approach using ultra-high performance liquid chromatography-diode array detection-quadrupole time of flight mass spectrometry (UHPLC-DAD-QTOFMS) providing both accurate mass full-scan mass spectrometry (MS) and tandem high resolution MS (MS/HRMS) data. The methodology was demonstrated on compounds from bioactive marine-derived strains of Aspergillus, Penicillium, and Emericellopsis, including small polyketides, non-ribosomal peptides, terpenes, and meroterpenoids. The MS/HRMS data were then searched against an in-house MS/HRMS library of ~1300 compounds for unambiguous identification. The full scan MS data was used for dereplication of compounds not in the MS/HRMS library, combined with ultraviolet/visual (UV/Vis) and MS/HRMS data for faster exclusion of database search results. This led to the identification of four novel isomers of the known anticancer compound, asperphenamate. Except for very low intensity peaks, no false negatives were found using the MS/HRMS approach, which proved to be robust against poor data quality caused by system overload or loss of lock-mass. Only for small polyketides, like patulin, were both retention time and UV/Vis spectra necessary for unambiguous identification. For the ophiobolin family with many structurally similar analogues partly co-eluting, the peaks could be assigned correctly by combining MS/HRMS data and m/z of the [M + Na]⁺ ions.     

不同品种亚麻籽脂肪酸含量的GC—MS分析

对35份不同品种的亚麻籽,用无水乙醚提取亚麻籽油,经皂化、甲酯化处理,采用气相色谱一质谱（GC—MS）联用技术对其脂肪酸含量进行测定。结果表明,亚麻籽油中的平均脂肪酸含量顺序为亚麻酸（41．62％）〉油酸（25．87％）〉亚油酸（17．18％）〉硬脂酸（6．59％）〉棕榈酸（6．46％）,不饱和脂肪酸含量高达85％。     

神农香菊花、茎和叶香气成分的组成分析

【目的】对神农香菊花、叶、茎的香气成分进行测定及比对分析,为研究和利用神农香菊独特的芳香性状提供理论基础。【方法】采用静态顶空吸附结合直接热脱附法-气相色谱/质谱联用(DTD-GC/MS)技术,对神农香菊花、叶、茎中的挥发性成分进行分析,用保留指数辅助定性及峰面积归一法对香气成分的相对含量进行测定及比对分析。【结果】神农香菊花朵中检测出的挥发物种类最多,共72种,其中同时存在于花、叶、茎香气中的挥发物有55种。萜烯类化合物含量在花、茎、叶香气中均占到总挥发物成分的80%以上,其中侧柏酮含量最高(50%),其他含量大于1%的重要成分有樟脑、桉树脑、β-石竹烯和大根香叶烯等。神农香菊花朵释放的香气量最多,茎、叶次之。【结论】神农香菊香气主要由萜烯类化合物组成,其花、茎、叶香气组成相似,但各成分含量有所差异。     

液相色谱法和液相色谱-串联质谱法测定蔬菜中多菌灵等15种农药残留量的研究

[目的]建立蔬菜中多菌灵等15种农药残留检测方法。[方法]分别采用高效液相色谱法(HPLC)和液相色谱-串联质谱法(LC/MS/MS)对不同蔬菜中多菌灵等15种农药残留进行检测。[结果]2种试验检测方法,多菌灵等部分农药残留量检测结果存在一定差异,这是蔬菜样品基质干扰所致。[结论]LC/MS/MS方法质谱抗干扰能力强、稳定、可靠,使用简便快速、分析时间短;HPLC方法需要更好的方法优化才能得到更可靠的检测结果。     

脲醛树脂及三聚氰胺改性脲醛树脂对桉木热解液组分的影响

为了有效利用热解技术处理废弃人造板,采用气质联用技术对比分析桉木、添加质量分数10% 脲醛(UF)树 脂的桉木、添加质量分数10%三聚氰胺改性脲醛(MUF)树脂的桉木、UF 树脂、MUF 树脂的热解液组分。结果表 明:桉木热解液成分复杂,其中2,5-二甲基呋喃的相对含量达到27.56%,3-甲基-2-羟基-2-环戊烯-1-酮和4-(2-氧 代)-2-环己烯-1-酮的相对含量分别为7.04%和7.02%,2,6-二甲氧基苯酚的相对含量为9.48%。添加UF 树脂的 桉木热解液检测到含氮物质的相对含量比桉木热解液增加22.93%,该热解液有望用于肥料生产和土壤改良;添加 MUF 树脂的桉木热解液出现了木糖、丁内酯等桉木热解液中未检测到的产物。