Application Example - Determination of 1,3-Dioxane in Cosmetics (GC/MSD Method)

Introduction

The most common uses of dioxane are as a solvent, emulsifier, and detergent, etc., and it can be absorbed into the human body through the respiratory tract, digestive tract, and mucous membranes. High concentrations of dioxane have anesthetic and irritating effects on people, and can cause eye and upper respiratory tract irritation, accompanied by dizziness, headache, drowsiness, nausea and vomiting. According to the "Hygienic Standards for Cosmetics" (2007 edition) issued by the Ministry of Health, dioxane is a prohibited substance in cosmetics.

Experimental part

Chromatographic and Mass Spectrometry Conditions

Instrumentation: Agilent 7697A Headspace Sampler - 7890A GC/

5975C Single Quadrupole GC/MSD (HS-GC/MSD) Inlet temperature: 250 °C

Split Ratio: 10:1

Carrier Gas: Nitrogen, 2 mL/min

Column: Agilent DB-5MS, 30 m × 0.25 mm, 0.25 µm Oven: Ramp from 50 °C to 150 °C at 20 °C/min Source temperature: 230 °C

Quadrupole temperature: 150 °C

Interface temperature: 280 °C

Acquisition Mode Selected Ion Monitoring (SIM)

Characteristic ions (m/z) 87.0, 58.0, 59.0

headspace conditions

Carrier gas control: Gas inlet EPC Headspace temperature: 80 °C

Sample loop temperature: 120 °C

Transfer line temperature: 140 °C

Sample loop size: 1 mL

Vial size: 20 mL

Vial equilibration time: 30 min

Vial Pressure Value: 15 psi

Vial inflation rate: 50 mL/min

Injection duration: 0.5 min

Vial Shaker Setting: 18/min

Vial pressurized gas: Helium

Experimental results