The largest database of trusted experimental protocols

3 protocols using hplc grade tfa

1

Analytical-scale HPLC and SEC-MALS analysis

Check if the same lab product or an alternative is used in the 5 most similar protocols
Analytical-scale HPLC was performed with an Agilent 1200 series system on octadecyl carbon chain (C18)–bonded silica columns (5-μm pore size, 4.6 × 250 mm, 218TP54, Vydac). The solvent system was HPLC-grade H2O (W/0106/PB17, Fisher Scientific) and HPLC-grade acetonitrile (ACN; A/0627/PB17, Fisher Scientific). Buffer A consisted of HPLC-grade H2O containing 0.1% (v/v) HPLC-grade TFA (T/3258/04, Fisher Scientific), and buffer B consisted of 80% (v/v) ACN in HPLC-grade H2O containing 0.1% (v/v) TFA.
Mass spectrometry analysis was performed on the Agilent Series 1100 LC-MS system in positive mode of ESI. The solvent system was as follows. Buffer A consisted of LC-MS grade H2O (W/0112/17, Fisher Scientific) containing 0.1% (v/v) formic acid (06440, Fluka), and buffer B consisted of 80% (v/v) ACN in MS-LC–grade H2O containing 0.1% (v/v) formic acid. Data analysis was performed with LC/MSD ChemStation software.
SEC-MALS was performed on a Superdex 200 5/150 GL column (GE Healthcare) in SEC-MALS buffer (50 mmol/liter Tris-HCl (pH 7.4), 5 mm MgCl2, 1 mmol/liter CaCl2, 100 mm NaCl, and 100 mmol/liter tris(2-carboxyethyl)phosphine). Recombinant troponins were extensively dialyzed against SEC-MALS buffer before experiments. Light scattering and refractive index were measured on a Mini DAWN and OPTILAB DSP (Wyatt Technology, UK), respectively. Data were analyzed with custom-written software.
+ Open protocol
+ Expand
2

Spectroscopic Characterization of Chemical Compounds

Check if the same lab product or an alternative is used in the 5 most similar protocols
All reagents were purchased from commercial suppliers and used without further purification. 1H NMR spectra were recorded on Bruker 500 MHz spectrometer with CDCl3, CD3OD or DMSO-d6 as the solvent. 13C NMR spectra were recorded at 125 MHz. All coupling constants are measured in Hertz (Hz) and the chemical shifts (δH and δC) are quoted in parts per million (ppm) relative to TMS (δ 0), which was used as the internal standard. High resolution mass spectroscopy was carried out on an Agilent 6210 LC/MS (ESI-TOF). HPLC-MS analysis was performed using Agilent 6120 single quadrupole 1220 LCMS equipped with Zorbax SB-C18 column (4.6 x 50 mm, 1.8 micron). The purity of final compounds that underwent biological assessment were >95% as measured by HPLC-MS. Thin layer chromatography was performed using silica gel 60 F254 plates (Fisher), with observation under UV when necessary. Anhydrous solvents (acetonitrile, dimethylformamide, ethanol, isopropanol, methanol and tetrahydrofuran) were used as purchased from Aldrich. Burdick and Jackson HPLC grade solvents (methanol, acetonitrile and water) were purchased from VWR for HPLC and high-resolution mass analysis. HPLC grade TFA was purchased from Fisher. Compound synthesis and characterization are detailed in the Supporting Information.
+ Open protocol
+ Expand
3

Synthesis and Characterization of (Rac)-i-Talazoparib

Check if the same lab product or an alternative is used in the 5 most similar protocols
All reagents were purchased from commercial suppliers and used without further purification. 1H NMR spectra were recorded on an Agilent-Varian Mercury 400 MHz spectrometer with CDCl3, CD3OD or DMSO-d6 as the solvent. 13C NMR spectra are recorded at 100 MHz. All coupling constants are measured in Hertz (Hz) and the chemical shifts (δH and δC) are quoted in parts per million (ppm) relative to TMS (δ 0), which was used as the internal standard. High resolution mass spectroscopy was carried out on an Agilent 6210 LC/MS (ESI-TOF). HPLC-MS analysis was performed using Agilent 6120 single quadrupole 1220 LCMS equipped with Zorbax SB-C18 column (4.6 × 50 mm, 1.8 micron). The purity of final compounds that underwent biological assessment were >95% as measured by HPLC-MS. Thin layer chromatography was performed using silica gel 60 F254 plates (Fisher), with observation under UV when necessary. Anhydrous solvents (acetonitrile, dimethylformamide, ethanol, isopropanol, methanol and tetrahydrofuran) were used as purchased from Aldrich. Burdick and Jackson HPLC grade solvents (methanol, acetonitrile and water) were purchased from VWR for HPLC and high resolution mass analysis. HPLC grade TFA was purchased from Fisher.
The compound 2, (Rac)-i-Talazoparib, was synthesized using similar methods decribed for preparation of talazoparib (1) (WANG ET AL., 2011 ).
+ Open protocol
+ Expand

About PubCompare

Our mission is to provide scientists with the largest repository of trustworthy protocols and intelligent analytical tools, thereby offering them extensive information to design robust protocols aimed at minimizing the risk of failures.

We believe that the most crucial aspect is to grant scientists access to a wide range of reliable sources and new useful tools that surpass human capabilities.

However, we trust in allowing scientists to determine how to construct their own protocols based on this information, as they are the experts in their field.

Ready to get started?

Sign up for free.
Registration takes 20 seconds.
Available from any computer
No download required

Sign up now

Revolutionizing how scientists
search and build protocols!