x 150 mm, Intersil Ph-3 column, GL Sciences, Torrance, CA) held at 40°C. A gradient with two mobile phases was used: (A) water (LC-MS grade) with 0.1% v/v formic acid; (B) methanol (LC-MS grade) with 0.1% v/v formic acid, using a flow rate of 0.3 mL/min. The injection volume was 2 µL. Samples were analyzed in a fully randomized batch. The ion spray voltage was set at 4,500 V and the source temperature was 500°C. Period cycle time was 641 ms; accumulation time 80 ms; m/z scan range 50 -1200 Da. The collision energy was set at 35 V with a collision energy spread setting of 15 V, and a declustering potential of 80 V.