Sensitivity booster for mass detection enables unambiguous analysis of peptides, proteins, antibodies, and protein bioconjugates

2019 ◽  
Vol 55 (67) ◽  
pp. 9979-9982 ◽  
Author(s):  
Rohith Singudas ◽  
Neelesh C. Reddy ◽  
Vishal Rai

A chemical tag enhances peptide detection by multiple orders in mass spectrometry.

2018 ◽  
Vol 10 (4) ◽  
pp. 87
Author(s):  
Yahdiana Harahap ◽  
Norma Andriyani ◽  
Harmita .

Objective: To obtain an optimum and validated method for analyzing lercanidipine in plasma using Ultra Performance Liquid Chromatography of Tandem Mass Spectrometry (UPLC-MS/MS).Methods: The separation was carried out using 1.7μm (2.1 x 100 mm) Waters AcquityTM UPLC C18 column, a mobile phase of the 0.1% formic acid-methanol mixture (20:80 v/v) with isocratic elution, 30 °C column temperature, 0.2 ml/min flow rate and amlodipine as an internal standard. Mass detection was performed with a positive XBL TQD type Electrospray Ionization (ESI) in Multiple Reaction Monitoring modes. Lercanidipine was detected at m/z value of 612.11>280.27 and amlodipine was detected at m/z value 409.1>238.15. The optimum sample preparation method was a liquid-liquid extraction using 5 ml of n-hexane-ethyl acetate (50:50 v/v), vortex mixed for 3 min, centrifuged at 4000 rpm for 20 min, evaporated with nitrogen at 50 °C for 30 min, and the residue was reconstituted with 100 μl of mobile phase.Results: The method was linear in the range of 0.025-10 ng/ml with r ≥ 0.9986. Accuracy and precision within-run and between-run met the requirements with %diff and %CV, not exceeding ± 15% and not more than ± 20% for Lower Limit of Quantification (LLOQ) concentration.Conclusion: It was concluded that the developed method met the requirements of selectivity, carry over, stability, the integrity of dilution, and matrix effects under the Guideline on Bioanalytical Method Validation by the European Medicines Agency in 2011. 


Molecules ◽  
2019 ◽  
Vol 24 (2) ◽  
pp. 233 ◽  
Author(s):  
Huanyu Guan ◽  
Xiaomei Luo ◽  
Xiaoyan Chang ◽  
Meifeng Su ◽  
Zhuangzhuang Li ◽  
...  

Wen Luo Yin (WLY), a well-known traditional Chinese medicine formulation, has been used as a complementary therapy for the treatment of rheumatoid arthritis in clinical settings. However, the chemical constituents of WLY remain unclear. In this study, a high-performance liquid chromatography coupled with tandem mass spectrometry method was established to separate and comprehensively identify the chemical constituents of WLY. The analytes were eluted with a mobile phase of acetonitrile and 0.1% aqueous acetic acid. Mass detection was performed in both positive and negative ion mode. The MS/MS fragmentation pathways were proposed for the identification of the components. A total of 42 compounds including sesquiterpenes, alkaloids, biflavonoids, polyacetylenes, phenylpropanoids and acetylenic phenols were identified unambiguously or tentatively according to their retention times and mass behavior with those of authentic standards or literature data. The identification and structural elucidation of chemical constituents may provide important information for quality control and pharmacological research of WLY.


2018 ◽  
Vol 9 (1) ◽  
Author(s):  
Brian C. Searle ◽  
Lindsay K. Pino ◽  
Jarrett D. Egertson ◽  
Ying S. Ting ◽  
Robert T. Lawrence ◽  
...  

2017 ◽  
Vol 14 (9) ◽  
pp. 903-908 ◽  
Author(s):  
Ying S Ting ◽  
Jarrett D Egertson ◽  
James G Bollinger ◽  
Brian C Searle ◽  
Samuel H Payne ◽  
...  

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