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Quantitative Analysis of N-Nitrosodimethylamine (NDMA), N-Nitrosodiethylamine (NDEA), and -Nitroso-N-methyl-4-aminobutyric acid (NMBA) in Losartan Potassium Tablets by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry
Carlo Joson and Therese Margaret Villar
- This analytical method highlights a sensitive and robust procedure for the quantitation of NDMA, NDEA, and NMBA in Losartan Potassium Tablet by LCMS/MS. The procedure was validated according to ASEAN Harmonization Guidelines, USP General Chapters <1225> and <736>.
LOQ (Limit of Quantitation) of the method: 0.22 ng NDMA / mg of sample, 0.07 ng NDEA / mg of sample, and 0.22 ng NMBA / mg of sample
Validated Range: 3 ng/mL to 1000 ng/mL of NDMA with respect to 50 ng/mL standard concentration, 1 ng/mL to 1000 ng/mL of NDEA with respect to 50 ng/mL standard concentration, and 3 ng/mL to 1000 ng/mL of NMBA with respect to 50 ng/mL standard concentration.
Precision: %Relative standard deviation (RSD) of NDMA, NDEA, and NMBA of the 6 recoveries at 100% levels are 3.6, 3.9, and 2.2, respectively.
Accuracy: Mean % recoveries of NDMA and NMBA at 3 ng/mL, 50 ng/mL, and 100 ng/mL are within 81.5 ~ 102.6% and 92.3% ~ 108.3%, respectively, while % recoveries of NDEA at 1 ng/mL, 50 ng/mL, and 100 ng/mL are within 87.4% ~ 101.5%.
Experimental Information
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Objective/Scope
- In the Philippines, growing awareness of the risks posed by nitrosamine contamination is encouraging pharmaceutical manufacturers and regulators to strengthen safety measures in line with international standards. To support this effort, UNILAB, Inc. has developed and validated an in-house quantitative testing method using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC–LCMS/MS) to accurately detect and measure NDMA, NDEA, and NMBA in Losartan Potassium tablets. This initiative reflects the company’s commitment to combining scientific rigor with proactive risk management to safeguard product quality and, ultimately, protect public health.)
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Instrumentation
- Waters ACQUITY UPLC I-Class PLUS System with Xevo TQ-S micro Triple Quadrupole Mass Spectrometer
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Method Principle
- NDMA, NDEA, and NMBA analysis using reverse-phase UPLC with LCMS/MS detection
Please see attachment for the detailed description of the method:
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