Phthalates Analysis With Method GB 5009.271-2016 Using the Agilent 8890 GC and MSD with Agilent JetClean

Importance of the Topic

Monitoring phthalate contamination in food is essential because these plasticizers can migrate from packaging into consumables. Certain phthalates are known endocrine disruptors or potential carcinogens, posing risks to human health, particularly affecting reproduction and development. Ensuring low phthalate levels in food products safeguards consumer safety and complies with global regulatory standards.

Objectives and Study Overview

The study demonstrates the application of Chinese national method GB 5009.271-2016 for quantifying 19 phthalates in food matrices. It evaluates the performance of an Agilent 8890 gas chromatograph (GC) coupled to a 5977B mass selective detector (MSD) equipped with JetClean self-cleaning ion source. Key goals include assessing repeatability, sensitivity, linearity, detection limits, and compliance with the standard.

Methodology and Instrumentation

Samples were represented by standard mixtures: a 16-component phthalate mix (1,000 ng/µL) and single-component standards (DINP, DAP, DIDP). Calibration solutions covered 10–1,000 ng/mL for 17 phthalates, and 125–20,000 ng/mL for DINP/DIDP. Instrumental conditions followed GB 5009.271-2016:

• GC inlet: splitless at 280 °C, purge to split vent after 0.5 min
• Oven program: 60 °C (1.5 min), 20 °C/min to 220 °C (1 min), then 5 °C/min to 280 °C (4 min)
• Column: Agilent J&W HP-5ms, 30 m × 0.25 mm, 0.25 µm
• Carrier gas: helium, 1.2 mL/min constant flow
• MSD: JetClean ion source at 320 °C with 0.13 mL/min H₂ for self-cleaning, quadrupole at 180 °C, interface at 280 °C, SIM acquisition

Results and Discussion

Seventeen phthalates were analyzed simultaneously, with DINP and DIDP in a separate run. Retention time precision was below 0.013 % RSD; area precision for 50 and 1,000 ng/mL standards remained under 5 % RSD. For DINP and DIDP at 250 ng/mL, area RSDs were 8.1 % and 5.2 %, respectively; at 1,000 ng/mL they improved to ~2 %. Method detection limits (MDLs) for 17 phthalates were under 10 ng/mL; MDLs for DINP and DIDP were 60 and 37 ng/mL. Calibration curves exhibited excellent linearity (R²>0.995 for 17 compounds; R²>0.998 for DINP/DIDP).

Benefits and Practical Applications

The 8890 GC–5977B GC/MSD combination with JetClean offers high reproducibility, sensitivity, and robust matrix tolerance. It meets or exceeds GB 5009.271-2016 criteria for precision and detection limits, supporting quality control in food testing laboratories and facilitating compliance with national and international regulations.

Future Trends and Potential Applications

• Extension to real-sample analysis and diverse food matrices
• Integration with automated sample prep for high throughput
• Development of rapid screening methods using alternative detectors
• Miniaturization and portable GC/MS platforms for on-site monitoring

Conclusion

The Agilent 8890 GC coupled with the 5977B MSD and JetClean ion source achieves reliable, sensitive, and accurate phthalate quantitation according to GB 5009.271-2016. Excellent repeatability, low MDLs, and strong linearity confirm its suitability for routine food safety testing.

Reference

1. GB 5009.271-2016: Determination of Phthalates in Food.
2. Feng Shuang; Hom Brian J. Sensitive and Reproducible Phthalate Analysis using the Agilent 5977 Series GC/MSD, Application Note 5991-1810EN, 2013.