The future of targeted peptidomics

Targeted MS is becoming increasingly important for sensitive and specific quantitative detection of proteins and respective PTMs. In this article, Ceglarek et al. [Proteomics Clin. Appl. 2013, 7, 794–801] present an LC-MS-based method for simultaneous quantitation of seven apolipoproteins in serum specimens. The assay fulfills many necessities of routine diagnostic applications, namely, low cost, high throughput, and good reproducibility. We anticipate that validation of new biomarkers will speed up with this technology and the palette of laboratory-based diagnostic tools will hopefully be augmented significantly in the near future.     

The development of multiple reaction monitoring assays for liver-derived plasma proteins

There is wide interpatient variability in toxicity to chemotherapeutic drugs and a lack of routine clinical tests for prospectively identifying patients at risk of developing toxicity from chemotherapy. An empirically driven MS strategy has been developed to monitor liver-derived plasma proteins as potential biomarkers of early toxicity. Multiple reaction monitoring (MRM) has been used to assess 46 candidate peptides from 18 liver-derived proteins. Following an iterative process of assay design, optimisation and assessment we selected 29 MRM assays (median CV 4.6%, range 1.2-11.6%) and monitored changes in levels of plasma proteins from a small number of colorectal cancer (CRC) patients undergoing chemotherapy. We demonstrated MRM assay robustness, and show that patients undergo minor elevation in plasma proteins when profiled on Day 3 of the chemotherapeutic regime. The MRM assays were in general agreement with 2-D DIGE-based quantitation from the same patient samples. The data supports the application of MRM-based methods as facile, highly reproducible, medium-throughput techniques that warrant expanded investigation for clinical utility in identifying patients at risk of developing chemotoxicity.     

The rapid selecting of precursor ions and product ions of thirty-four kinds of pesticide for content determination by GC–EI/MS/MS

Pesticide residues caused great threat to human body health, and all countries protected the health of human body by specifying its upper limit. However, pesticide residues were generally very low, similar to trace analysis and as low as millionth or less, the content determination of pesticide residues was a troublesome problem. With the application and promotion of tandem mass spectrometry, it was able to do trace analysis. GC–EI/MS/MS was a common method for the determination of pesticide residues. The multiple reaction monitoring (MRM) mode was the most common quantitative method used in GC–EI/MS/MS. It has the characteristics of high sensitivity, good reproducibility, high accuracy, strong anti-interference and high ion flux. Multiple-twin precursor ions, product ions and collision energy of thirty-four pesticides were provided for MRM. It could play an important role in developing MRM method for the quantifying of 34 kinds of pesticide. Meanwhile, the development of MRM method for the quantifying of other compounds could also refer to this paper.     

A rapid method for simultaneous determination of triterpenoid saponins in Pulsatilla turczaninovii using microwave-assisted extraction and high performance liquid chromatography–tandem mass spectrometry

In the present study, a microwave-assisted extraction (MAE) and high performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) method was developed for the simultaneous determination of seven triterpenoid saponins in Pulsatilla turczaninovii. Operational conditions of MAE were optimized using a central composite design. Multiple-reaction monitoring was employed for quantification while switching the electrospray ion source polarity between positive and negative modes. Full validation of the method was carried out (linearity, precision, accuracy, limit of detection and limit of quantification). The results indicated that the method was rapid, specific and reliable. The developed method was successfully applied to determine the investigated compounds in nine batches of P. turczaninovii. These samples were collected in different seasons from the Liaoning province and varied greatly. The total triterpenoid saponins content was the highest in April, the seedling stage, and decreased from May to August. The contents of total triterpenoid saponins decreased significantly after the blooming period.     

超高效液相-质谱联用法测定化妆品中9种禁用激素

建立化妆品中非法添加的9种糖皮质激素的快速测定方法。采用超高效液相色谱-串联质谱法(UPLC-MS/MS),以ACQUITY UPLC~BEN C18色谱柱(50 mm×2.1 mm,1.7μm),流动相采用甲醇-水,电喷雾电离(ESI)联合相关信息扫描(IDA)与增强离子扫描(EPI)的扫描方式,对化妆品中非法添加的9种糖皮质激素成分进行快速定性分析,检测限低于0.4μg/m L。     

An improved LC-MS/MS method for the quantitation of acrylamide in processed foods

An improved liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of acrylamide in processed foods. The homogenized samples, spiked with ¹³C₃-acrylamide as an internal standard, were extracted with water and centrifuged. D₅-3-chloropropanediol as a recovery standard was added to 1-ml aliquots, and the sample was purified with a C₁₈-cartridge column. The extract was directly analyzed using LC-MS/MS without derivatization. The ion transitions of 72–55 m/z (acrylamide), 75–58 m/z (¹³C₃-acrylamide), and 116–98 m/z (d₅-3-chloropropanediol) were found to be the most reliable for the identification and quantification of acrylamide in multiple reaction monitoring. The limit of quantification for acrylamide, defined as a signal-to-noise ratio of 10:1, was 2 μg/kg. The use of d₅-3-chloropropanediol minimized the effects of variation in the sample matrixes and increased the quality of analysis. This method could be applied to the quantification of acrylamide in processed foods.     

常规定量的理想选择——安捷伦6420三重串联四极杆液质联用仪

本文主要介绍了安捷伦6420三重串联四极杆液质联用仪的的性能特点。重点介绍了6420的可升级功能,触发式多反应监测功能和动态多反应监测功能,以及这些功能所能带来的优势。并指出了6420所针对的应用领域。     

声像管理系统――播出系统设计方案详解

随着各行业信息化建设进程的加快,多媒体资源的数字化管理工作被越来越多的单位所重视,为了解决行业用户大量多媒体资料数字化保存、检索和共享发布所面临的问题,提出了声像管理系统。结合某单位在声像管理系统方面的应用实践,详细分析了声像管理系统中播出环节的系统设计、网络架构、业务功能。该媒资系统的实践给媒资系统构建方法,甚至业务的拓展以及异构系统间的互通提供了很好的应用经验。     

Study of flavonoids in aqueous spinach extract using positive electrospray ionisation tandem quadrupole mass spectrometry

The presence of three flavonols (quercetin, kaempferol, myricetin) and two flavones (apigenin, luteolin) were investigated in the extract of fresh spinach leaves. Aqueous spinach extracts were prepared with a leaf/water ratio of 1:2 at 80 °C for 30 min stirring. Ferric ammonium sulphate method was used for measuring total polyphenols in the extracts and expressed as catechins and tannic acid equivalents. The flavonoids glycosides in the extract were hydrolysed to their aglycons with 1.2 M HCl in boiling 50% water methanol solution. The resulting aglycons were identified and quantified by a C18 reverse phase high-performance liquid chromatography (RP-HPLC). Furthermore, the results were confirmed by HPLC coupled to an electrospray ionisation tandem triple-quadrupole mass spectrometer ESI-MS performing low-energy collision induced dissociation (CID-MS/MS) in the collision cell (HPLC-ESI-MS/MS). Analyses were made in the multiple reaction monitory (MRM) mode. Results showed that total polyphenols contents in fresh spinach leaves were 270 mg kg⁻¹ and 390 mg kg⁻¹ as tannic acid and catechin equivalents, respectively, in which, major flavonoids aglycons were apigenin (170 mg kg⁻¹), quercetin (50 mg kg⁻¹) and kaempferol (30 mg kg⁻¹).     

高效液相色谱-串联质谱法测食品中的赭曲霉毒素A

研究建立高效液相色谱-串联质谱联用技术检测食品中赭曲霉毒素A的方法。根据不同样品,用甲醇-2%碳酸氢钠溶液(60:40,V/V)或甲醇-水(80:20,V/V)提取样品中的赭曲霉毒素A,经OchraTest亲和柱净化,以甲醇-5mmol/L(含0.1%甲酸)乙酸铵为流动相,采用正离子模式对赭曲霉毒素A进行检测。结果回收率在82.3%～98.5%之间,检出限为0.1μg/kg。该方法适用不同基质样品,准确性好、灵敏度高、抗干扰能力强,方法检出限可满足欧盟等最新限量要求。