基质辅助激光解析/电离飞行时间质谱(MALDI-TOF MS)在微生物鉴定中的应用*

基质辅助激光解析/电离飞行时间质谱(MALDI-TOF MS)是一种新型软电离生物质谱,具有检测速度快、操作简便、结果准确等优点,目前已成为可靠的微生物快速鉴定技术。就工作流程而言,与常规生化方法相比,MALDI-TOF MS可以将微生物鉴定的时间缩短为一天甚至更短。对于具有抗生素耐药性的微生物,使用MALDI-TOF MS鉴定也有很好的准确性。在病毒鉴定中,MALDI-TOF MS也可以发挥作用,已有报道将MALDI-TOF MS和机器学习(ML)分析方法结合来检测鼻拭子中SARS-CoV-2。此外,MALDI-TOF MS还可用于细菌的无光谱库鉴定。目前,MALDI-TOF MS正通过与其他技术(例如傅里叶红外光谱FTIR)相结合进一步扩大微生物鉴定范围。     

适用于本科教学的BET比表面测定实验

采用自组装的流动吸附仪建立了基于BET吸附原理的快速测定固体比表面积的实验方法(单点法),对同一活性炭样品,在多功能气体吸附系统上进行对照实验(多点法)。实验结果表明,采用流动吸附仪测定比表面积方便易行,数据稳定可靠,实验教学效果良好。本文介绍这一特色实验,期望对从事物理化学实验教学的同行有所助益。     

Ultra‐performance liquid chromatography coupled with electrospray ionization/quadrupole time‐of‐flight mass spectrometry for the rapid analysis of constituents in the traditional Chinese medical formula Danggui San

In this work, ultra‐performance LC with ESI quadrupole TOF‐MS (UPLC–ESI‐Q‐TOF‐MS) and automated MetaboLynx analysis was used to rapidly separate and identify the chemical constituents of Danggui San, a traditional Chinese medical formula. The analysis was performed on a Waters UPLC BEH C₁₈ column using a gradient elution system. A hyphenated ESI and Q‐TOF analyzer was used for the determination of the accurate mass of the protonated or deprotonated molecule and fragment ions in both positive and negative modes. Based on retention times, accurate mass, and the mass spectrometric fragmentation characteristics, a total of 47 compounds distributed over the chemical groups of phthalides, flavonoids, monoterpene glycosides, sesquiterpenoids, phenolics, and alkaloids, were simultaneously separated within 18 min and identified or tentatively elucidated in Danggui San for the first time. UPLC–ESI‐Q‐TOF‐MS analysis revealed the complexity of the chemical composition of this formula. The method developed is rapid, accurate, reliable, and highly sensitive to characterize the chemical constituents of Danggui San.     

Compounds with inhibitory activity on peristalsis from the seeds of Holarrhena antidysenterica

Eight compounds were isolated from the seeds of Holarrhena antidysenterica Wall.ex A.DC. On the basis of physico-chemical properties and spectroscopic data, holarrhenanan (1) was identified as a new compound, compounds 2–3 were isolated from H. antidysenterica for the first time, and five known compounds were also obtained. Inhibitory effects of some compounds and extracts to the intestinal peristalsis were evaluated. Results showed that the extracts and compounds 4, 6 exhibited remarkable inhibitory effects with tension inhibition rate of 32.77, 32.77% and amplitude inhibition rate of 59.51, 55.98%, respectively on the vitro rabbit intestinal peristalsis.     

临界点二级相变的有限时间热力学逼近

应用内可逆卡诺循环的方法,导出了各种物质在临界点附近可逆与不可逆二级相变普遍适用的比热跃变公式以及广义的爱伦菲斯特方程。对简单(P,V,T)系统、超导、电介质顺电一铁电二级相变进行了应用讨论。     

原油饱和烃指纹的内标法分析

采用内标法建立了原油中正构烷烃、生物标志物(甾、萜烷类)的分析方法。确定了样品前处理方法和组分定性定量方法。讨论了柱层析分离能力。结果表明,所有饱和烃组分均流入第一部分流出液F1中,分离能力较为满意。对48种甾、萜烷类生物标志物组分以及姥鲛烷、植烷和正构烷烃等进行了定性确认,定性化合物数量多,信息量大,易于据此进行可靠的油指纹分析鉴别。32个正构烷烃组分相对标准差为1.2%～7.4%;45个生物标志物组分相对标准偏差为2.5%～9.2%。分析精密度较好,满足油指纹鉴别需要。正构烷烃回收率为73%～116%;生物标志物为84%～106%;回收率结果较为满意。正构烷烃方法检出限为7.0μg/g;生物标志物为0.65μg/g,满足原油样品分析要求。通过本方法对自不同和相同平台的原油样品进行饱和烃浓度分析,并采用浓度数据进行鉴别,结果与实际情况相符。     

氢化诺卜醇及其烷基醚的合成与表征

由β-蒎烯与多聚甲醛反应制得诺卜醇,然后用Ni(R)催化氢化制得氢化诺卜醇(ROH),再将氢化诺卜醇与亚硫酰氯反应制得氢化诺卜基氯(RCl),由RCl分别与6种醇钠反应合成了6种氢化诺卜基烷基醚,各产物的得率均在92%以上,GC纯度95%以上。各产物都用IR,1H NMR,13C NMR与MS进行了结构表征。     

Isolation and identification of nondestructive desulfurization bacterium

A nondestructive desulfurization microorganism has been isolated. The metabolism product analyses show that the strain can be a kind of biocatalyst to oxidize dibenzothiophene (DBT) into 2-hydroxydiphenyl (HBP), therefore the sulfur in DBT is removed selectively. The 16SrRNA information, cell wall analysis, physical, biochemical properties and morphological properties suggest that the isolated strain is Rhodococcus erythropolis. The strain can grow in the basal salts medium (BSM) that DBT concentration is no more than 10 mmol/L, and the optimal DBT concentration for growth is 1 mmol/L, however, the optimal DBT concentration for desulfurization is 0.5 mmol/L. The further research shows that the strain can also desulfur some other or-ganosulfur-containing compounds such as thianaphthene, phenyl sulfide and 4,6-dimethyldiben-zothiophene (4,6-DMDBT).     

钳蝎毒中抗癫痫肽、镇痛肽和抗肿瘤肽的快速同时分离和鉴定

采用Shim-Pack WCX-1型阳离子交换高压色谱柱对中国东亚钳蝎全蝎毒进行了分离，在鉴定了其中的抗癫痫肽、镇痛肽和抗肿瘤肽活性峰的基础上，应用Shim-Pack DIOL-300型凝胶排阻高压色谱柱对它们进行了进一步分离和鉴定，可以得到较纯的3种多肽。在高压色谱所提供的全蝎毒分离信息的基础上，应用与Shim-Pack WCX-1色谱柱具有相同交换基团的、具有较大吸附容量的CM Sepharose CL-6B软胶介质在低压色谱上对全蝎毒进行了分离，并分别对其中的抗癫痫肽、镇痛肽和抗肿瘤肽进行了鉴定。     

新型除草剂丙酯草醚A环14C均标记合成和鉴定

以U-¹⁴C-对氨基苯甲酸为前体, 通过酯化、缩合、还原和取代四步反应获得了A环¹⁴C均标记的丙酯草醚, 用PHPLC对其进行纯化. 采用HPLC-MS(ESI), MS(EI)和¹H NMR验证了其结构, 通过HPLC(外标法)确定其化学纯度大于98%; HPLC-LSC和TLC-IIA两种方法分析表明, 其放射化学纯度大于98%, 其比活度为1.089±0.011 mCi/mmol. 合成的化学收率和放化收率均为53%.