Development of quantitative analytical method for volatile thiol compound with LC-ESI-MS as nonvolatile derivative by integrating a thiol-specific derivatization

Author(s):  
Yusuke Kawano ◽  
Kengo Suzuki ◽  
Iwao Ohtsu

Abstract Generally, volatile thiols are hard to be measured with ESI (electrospray ionization)-type LC-MS due to the volatility. Therefore, we here evaluated the pretreatment of their S-bimanyl derivatization by monobromobimane to enable the detection as nonvolatile derivative. Consequently, we successfully developed the convenient and efficient method through the quantitative analysis of 2-furanmethanethiol (volatile thiol odorant of coffee aroma) in coffee bean.

2016 ◽  
Vol 99 (5) ◽  
pp. 1273-1278 ◽  
Author(s):  
Shaoying Liu ◽  
Jicai Fan ◽  
Xihui Huang ◽  
Quan Jin ◽  
Guonian Zhu

Abstract A simple method was developed for the determination of sterigmatocystin in infant cereals. The method consists of a quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction approach and cleanup with an SPE HLB cartridge. After purification for separation and quantification of sterigmatocystin, HPLC with UV detection and diode-array detection (DAD) was used at sterigmatocystin levels >10 μg/kg, whereas ultra-performance LC with electrospray ionization (ESI) and tandem MS (MS/MS) was used at levels <10 μg/kg. The compound was determined by UV-DAD at 325 nm and by ESI-MS/MS in the positive ionization mode. Good r2 values (≥0.99) were found with both UV-DAD and ESI-MS/MS, and satisfactory recoveries (84.8–96.2%) of sterigmatocystin in infant cereals were demonstrated, with RSD values ≤11.43%. The developed analytical method was used for the determination of sterigmatocystin in infant cereals from Hangzhou, China.


Molecules ◽  
2019 ◽  
Vol 24 (19) ◽  
pp. 3463
Author(s):  
Miao Tian ◽  
Chunjuan Yang ◽  
Jing Yang ◽  
Hongrui Dong ◽  
Lu Liu ◽  
...  

In this study, the constituents of a Corydalis bungeana Turcz extract were qualitatively analyzed using gradient elution with a mobile phase of 0.2% acetic acid and acetonitrile. We obtained comprehensive insight into the constituents of C. bungeana Turcz extracts through the quantitative analysis of 14 compounds by comparison with authentic reference standards, and tentatively identified an additional 44 compounds through electrospray ionization mass spectrometry (ESI–MS) and tandem MS detection. The separation was successfully achieved using an Agilent SB-C18 column (1.8 µm, 150 × 2.1 mm; Agilent, Santa, CA, USA). A tandem quadrupole spectrometer was operated in either full-scan mode or multiple reaction monitoring (MRM) for the qualitative and quantitative analyses of the constituents, respectively. Validation data (inter-day and intra-day combined) for accuracy and precision ranged from −4.80% to 4.73%, and 0.30% to 4.97%, respectively. An ultrahigh performance liquid chromatographic–ESI–tandem MS (UHPLC–ESI–MS/MS) method for qualitative of C. bungeana Turcz (C. bungeana) extract and the quantification of 14 alkaloids, namely, A–N, was developed and validated. Quantitative analysis involved gradient elution with a mobile phase of 0.1% acetic acid and methanol for 45 min. The separation was successfully achieved using a Waters SB-C18 column (1.8 µm, 100 mm × 2.1 mm, Waters, Milford, Massachusetts, USA). The repeatability and stability of the method also met USFDA criteria with CV values lower than 5%. The limit of detection of the 14 alkaloids ranged from 9.74 to 13.00 ng/mL, whereas the linearities of the standard curves were between 0.9991 and 0.9995. In total, 15 commercial samples from 11 different sources were analyzed.


The Analyst ◽  
2015 ◽  
Vol 140 (8) ◽  
pp. 2623-2627 ◽  
Author(s):  
Gongyu Li ◽  
Jiying Pei ◽  
Yue Yin ◽  
Guangming Huang

Enhanced corona discharge was employed for in-spray dissociation of disulfide bonds, facilitating disulfide-containing peptide sequencing with ESI-MS/MS.


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