Lcms 8050 triple quadrupole lc ms ms

The amounts of TKIs were determined with a LCMS-8050 triple quadrupole LC-MS/MS (Shimadzu, Kyoto, Japan) coupled to an LC-30A system (Shimadzu) using an ACQUITY UPLC BEH C18 column (130 Å, 1.7 μm, ID 2.1 mm × 50 mm; Waters Corporation, MA, USA) at 40 °C. The mobile phase was composed of a mixture of 0.1% formic acid in water (pH 3.0) and 0.1% formic acid in acetonitrile at the flow rate of 0.2 mL/min. The mass numbers of the molecular and product ions for each compound were as follows: crizotinib (449.9 → 260.2, CE −24 V), gefitinib (447.2 → 128.2, CE −23 V), imatinib (494.3 → 394.3, CE −28 V) pazopanib (438.1 → 357.2, CE −35 V), sorafenib (464.9 → 252.0, CE −21 V), and sunitinib (399.2 → 283.0, CE −29 V). Labsolutions software (version 5.89, Shimadzu) was used for data manipulation. The detection limit was 10 nM for each compound.

The concentration of 1-MNA was determined using an LC-MS-8050 triple quadrupole LC-MS/MS (Shimadzu, Kyoto, Japan) coupled to an LC-30A system (Shimadzu). Chromatography was performed on an InertSustain amide column (ID 2.0 mm × 50 mm; GL Sciences) at 40 °C by means of step-gradient elution (flow rate, 0.4 mL/min) as follows: 0 to 2.0 min, 13% A/87% B; 2.0 to 2.5 min, 13% A/87% B to 50% A/50% B; 2.5 to 4.0 min, 50% A/50% B; 4.0 to 4.5 min, 50% A/50% B to 13% A/87% B; and 4.5 to 7.0 min, 13% A/87% B. A was water containing 0.1% formic acid and B was acetonitrile containing 0.1% formic acid. The mass numbers of the molecular and product ions for each compound were as follows: 1-MNA (137.2 → 94.2, CE − 22.0 V) and 1-MNA-d3 (Toronto Research Chemicals, North York, Canada) (140.0 → 97.2, CE −22.0 V). Lab solutions software (version 5.89, Shimadzu) was used for data manipulation. The detection limit was 10 ng/mL for each compound.