Usp Residual Solvents Analytical Method
Residual solvents
Identification and control of the residual solvents (USP 32(467), page 181
Determination by gas chromatography with mass detector and headspace sampler
Conditions of the chromatograph Agilent 7890A (LCTG CGMS): * Column DB-624 30m 0.25 mm 1.4µ (CG-2) * Injector temperatura: 160ºC * Flux: 1.0 ml/min * Split: 5:1 * Carrier gas: Helium * Time per test: 30.6 min
Conditions of the detector 5975C inert MSD * Data adquisition mode: Scan/SIM * Mass: from 30 to 200 * Threshold 75 * Temperature of the source: 230ºC * Quadrupol temperature: 150ºC
Conditions of the Headspace G1888 (LCTG HSS02) * Oven temperature: 85ºC * Loop temperature: 100ºC * Transfer line temperature: 120ºC * Vial equilibrium time: 30 min * Vial pressurization time: 0.15 min * Loop equilibrium time: 0.05 min * Loop fill up time: 0.2 min * Injection time: 0.5 min * Loop size: 1ml * GC Cycle time: 37 min
Standards and sample preparation
_ Class 1 standard reference solution: Transfer 1 ml of the USP reference standard for residual solvent class 1 to a 100 ml volumetric flask. Add 9 ml of DMSO. Dilute to volume with water and agitate. Transfer 1 ml of this solution to a 100 ml volumetric flask, dilute to volume and agitate. Transfer 10.0ml of this solution to a 50ml volumetric flask dilute to volume and agitate.
_ Class 1 residual solvents standard: Transfer 1 .0ml of the reference solution to a headspace vial of 10ml. Add 5.0ml of water, close and agitate
_ Class 2 standard reference solution: Transfer 1 ml of the USP reference standard mixture A for residual solvent class 2 to a 50 ml volumetric flask.Dilute to volume with water and agitate. This is the reference standard A. Transfer 1 ml of the USP reference standard mixture B for residual solvent class 2 to a 50 ml volumetric flask.Dilute to volume with water and agitate. This is the reference standard B.
_ Class 2 residual solvents
Identification and control of the residual solvents (USP 32(467), page 181
Determination by gas chromatography with mass detector and headspace sampler
Conditions of the chromatograph Agilent 7890A (LCTG CGMS): * Column DB-624 30m 0.25 mm 1.4µ (CG-2) * Injector temperatura: 160ºC * Flux: 1.0 ml/min * Split: 5:1 * Carrier gas: Helium * Time per test: 30.6 min
Conditions of the detector 5975C inert MSD * Data adquisition mode: Scan/SIM * Mass: from 30 to 200 * Threshold 75 * Temperature of the source: 230ºC * Quadrupol temperature: 150ºC
Conditions of the Headspace G1888 (LCTG HSS02) * Oven temperature: 85ºC * Loop temperature: 100ºC * Transfer line temperature: 120ºC * Vial equilibrium time: 30 min * Vial pressurization time: 0.15 min * Loop equilibrium time: 0.05 min * Loop fill up time: 0.2 min * Injection time: 0.5 min * Loop size: 1ml * GC Cycle time: 37 min
Standards and sample preparation
_ Class 1 standard reference solution: Transfer 1 ml of the USP reference standard for residual solvent class 1 to a 100 ml volumetric flask. Add 9 ml of DMSO. Dilute to volume with water and agitate. Transfer 1 ml of this solution to a 100 ml volumetric flask, dilute to volume and agitate. Transfer 10.0ml of this solution to a 50ml volumetric flask dilute to volume and agitate.
_ Class 1 residual solvents standard: Transfer 1 .0ml of the reference solution to a headspace vial of 10ml. Add 5.0ml of water, close and agitate
_ Class 2 standard reference solution: Transfer 1 ml of the USP reference standard mixture A for residual solvent class 2 to a 50 ml volumetric flask.Dilute to volume with water and agitate. This is the reference standard A. Transfer 1 ml of the USP reference standard mixture B for residual solvent class 2 to a 50 ml volumetric flask.Dilute to volume with water and agitate. This is the reference standard B.
_ Class 2 residual solvents