Phthalates Analysis in Toys Using Agilent 5977E GC/MS

Importance of the Topic

Phthalates serve as plasticizers in PVC and appear in consumer goods such as toys. Due to toxicological concerns affecting liver, hormonal and reproductive systems, regulations limit their presence in children’s products. Accurate analysis is essential for enforcement and protection of vulnerable populations.

Objectives and Study Overview

This study evaluates the Agilent 5977E GC/MS system for quantifying six regulated phthalates in PVC toys following GB/T 22048-2008 guidelines, focusing on calibration, linearity, repeatability, and system stability.

Methodology

Toy samples were ground and Soxhlet-extracted with dichloromethane at 60–80 °C for six hours. Extracts were concentrated and diluted. Calibration standards ranged 0.5–10 mg/L for DBP, BBP, DEHP, DNOP and 5–100 mg/L for DINP, DIDP. Samples were injected in split mode (5:1) with a 290 °C inlet, helium at 1.2 mL/min, and oven program from 180 °C to 280 °C.

Used Instrumentation

• Agilent 5977E GC/MSD with electron impact ionization
• Agilent 7650A automatic liquid sampler
• Split/splitless inlet with ultra-inert liner
• Agilent HP-5ms UI column (30 m × 0.25 mm, 0.25 μm)
• MS detection in full scan mode (50–550 u)

Main Results and Discussion

The total ion chromatogram achieved clear separation of six phthalates with retention times from 4.2 to 12 minutes. Raising the ion source temperature from 230 °C to 300 °C improved linearity for high boiling compounds, achieving R² > 0.999. Repeatability tests at 5 mg/L and PVC sample injections yielded RSDs below 5%, confirming excellent system stability.

Benefits and Practical Applications

The method fulfills international regulatory requirements and provides a cost-effective, precise solution for routine quality control and compliance testing of phthalates in consumer and environmental samples.

Future Trends and Potential Applications

Ongoing regulatory tightening may demand lower detection limits and analysis of additional plasticizers. Integration with automated sample preparation and high-throughput GC/MS protocols will enhance laboratory efficiency and expand multi-residue capabilities.

Conclusion

The Agilent 5977E GC/MS system offers a reliable and economical approach for analyzing six regulated phthalates in toys, demonstrating excellent linearity, repeatability, and stability as per GB/T 22048-2008 standards. This method is well-suited for regulatory compliance and quality assurance.

Reference

• Official Journal of the European Communities Decision 98/815/EC, 1999
• U.S. Consumer Product Safety Improvement Act, 2008
• GB/T 22048-2008: Determination of phthalate plasticizers in PVC toys