High Sensitive and Accurate Analysis of Nitrosamines

Significance of the Topic

Trace levels of nitrosamines in pharmaceutical products, environmental waters and foodstuffs pose a significant health risk due to their carcinogenic potential. Reliable, sensitive and fast analytical methods are essential for routine monitoring, regulatory compliance and protection of public health.

Aim and Overview of the Study

This application note describes the development of a high-sensitivity, high-accuracy GC-MS/MS method for the simultaneous quantification of five common nitrosamines: NDMA, NDEA, NEIPA, NDIPA and NDBA. The study demonstrates method performance, including separation characteristics, detection limits and quantitation range, using Shimadzu’s GCMS-TQ™ 8050 NX system.

Methodology

The analytical procedure employs splitless injection (2 µL) at 250 °C with high-pressure injection for 1.5 min. Separation is achieved on a 30 m × 0.25 mm I.D., 1.4 µm SH-1-624Sil MS column with a temperature program: 50 °C (1 min) ramped at 20 °C/min to 250 °C (3 min). Carrier gas is controlled by linear velocity at 39.7 cm/s. The triple quadrupole MS operates in MRM mode using electron ionization. Collision energies and characteristic transitions are optimized for each analyte.

Used Instrumentation

• Gas chromatograph–triple quadrupole mass spectrometer: Shimadzu GCMS-TQ 8050 NX
• Autosampler: AOC-20i+s Plus
• Column: SH-1-624Sil MS (30 m × 0.25 mm I.D., 1.4 µm; P/N 221-75962-30)
• Insert liner: Splitless deactivated liner with low wool

Main Results and Discussion

Baseline separation of all five nitrosamines is achieved within 10 minutes. Calibration curves exhibit excellent linearity (r² > 0.999) over the tested concentration ranges. Limits of detection (LODs) are in the low parts-per-trillion range, ensuring detection well below regulatory thresholds. Repeatability and accuracy meet stringent QA/QC requirements, with recovery rates above 90%.

Benefits and Practical Applications of the Method

• Rapid analysis suitable for high-throughput laboratories
• Ultra-low detection limits for stringent regulatory compliance
• Robust quantitation across a broad concentration range
• Applicability to pharmaceutical, environmental and food testing

Future Trends and Potential Applications

Advances may include automated sample preparation workflows, coupling with high-resolution mass spectrometry for non-targeted nitrosamine screening, and miniaturized GC-MS systems for on-site monitoring. Integration of green chemistry approaches for solvent reduction is also anticipated.

Conclusion

The described GC-MS/MS method on the Shimadzu GCMS-TQ 8050 NX platform delivers high sensitivity, accuracy and throughput for the determination of nitrosamines. Its robust performance supports critical QA/QC tasks and regulatory monitoring in diverse matrices.

Reference

Application News 01-00242 (JP, ENG), Shimadzu Corporation, First Edition: Sep. 2022