Improved Analytical Methods for Determination of Residues of Nitrapyrin and 6-Chloropicolinic Acid in Different Crop Matrices by Liquid Chromatography-Tandem Mass Spectrometry
Novel analytical methods were developed for the determination of nitrapyrin and 6-chloropicolinic acid (6-CPA) residues in agricultural products. Nitrapyrin was extracted with hexane: toluene (1:1, v/v) and 6-CPA with 0.1 N sodium hydroxide (NaOH). For nitrapyrin, samples were cleaned with silica solid phase extraction (SPE) and for 6-CPA with C18 or carbon SPE. Analysis was performed by liquid chromatography-tandem mass spectroscopy (LC-MS/MS) with external calibration (0.010 to 0.0010 μg？mL？1 for nitrapyrin and 0.0050 to 0.00025 μg？mL？1 for 6-CPA). Recoveries for nitrapyrin and 6-CPA were 68% - 102% and 66% - 90%, respectively. Nitrapyrin was detected in celery and onion (<0.020 to 0.15 μg？g？1) and 6-CPA in onion, mustard greens and lettuce (<0.050 - 0.19 μg？g？1). Lower level method validation (LLMV) for nitrapyrin and 6-CPA was 0.020 μg？g？1 and 0.050 μg？g？1, respectively. The methods presented in this study are robust and were utilized for the registration of nitrapyrin on agricultural commodities in the United States.
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