Sil 30acxr

Analyses of all samples were performed on a UHPLC system (Shimadzu, Kyoto, Japan) which is composed of a solvent delivery system LC-3AD, an autosampler SIL30ACXR, a column oven CTO-30AC, a degasser DGU-20A3, and a controller CBM-20A. The separation was conducted on an UHPLC Agilent column Zorbax EcLipse Plus C18 at a flow rate of 0.3 mL/min (1.8 μm, 100 mm × 2.1 mm). During the analysis, the column temperature was maintained at 40 °C. The mobile phase is made of water with 0.1% formic acid (A) and acetonitrile with 0.1% formic acid (B). The elution program was set as follows: 0–15 min, 10%–95% B; 15.01–19 min, 10% B. A triple TOFM X500R system equipped with a Duo Spray source (AB SCIEX, Foster City, CA, USA) was used to conduct the MS analysis in the negative electrospray ion mode. The parameters of electrospray ionization (ESI) were set as follows: ion spray voltage: −4500 V; curtain gas: 35 psi; ion source temperature: 550 °C; declustering potential (DP): −100 V, nebulizer gas (GS 1): 55 psi, and heater gas (GS 2): 55 psi. m/z 100–1600 Da was used for the MS scan. Data analysis were performed by the Peak View® 1.4 software (AB SCIEX Foster City, CA, USA).