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...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 (−1) and 6-CPA in onion, mustard greens and lettuce (−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.展开更多
文摘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 (−1) and 6-CPA in onion, mustard greens and lettuce (−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.
