Jadhav Manjusha, Thekkumpurath Ahammed Shabeer, Nakade Mayura, Gadgil Manasi, Oulkar Dasharath, Arimboor Ranjith, Ramakrishna Menon, Banerjee Kaushik
Indian Council of Agricultural Research, National Research Centre for Grapes, National Referral Laboratory, PO Manjri Farm, Pune 412 307, Maharashtra, India.
Government of India, Ministry of Commerce & Industry, Spices Board, Cochin 682 025, Kerala, India.
J AOAC Int. 2017 May 1;100(3):603-609. doi: 10.5740/jaoacint.17-0061.
A QuEChERS technique-based sample preparation method was optimized and validated in small cardamom to monitor the residues of 154 pesticides by LC with tandem MS. The proposed multiresidue method involved soaking powdered cardamom (2 g) in water (8 mL) for 30 min, followed by extraction with acetonitrile (10 mL). Cleanup by dispersive SPE was performed using primary secondary amine (25 mg/mL), C18 (25 mg/mL), and anhydrous magnesium sulfate (150 mg/mL). The method was validated as per the SANTE/11945/2015 guidelines at 5, 10, 50, and 100 ng/g spiking levels, and most of the analytes showed recoveries between 70 and 120% (with RSDs ≤20%). The LOQ of ≤10 ng/g was achieved for almost 90% of the target pesticides. The measurement uncertainties were evaluated at 100 ng/g, and the global uncertainty values were below 22% for all the analytes.
优化并验证了一种基于QuEChERS技术的小豆蔻样品制备方法，用于通过液相色谱-串联质谱法监测154种农药的残留。所提出的多残留方法包括将小豆蔻粉末（2 g）在水（8 mL）中浸泡30分钟，然后用乙腈（10 mL）萃取。使用伯仲胺（25 mg/mL）、C18（25 mg/mL）和无水硫酸镁（150 mg/mL）通过分散固相萃取进行净化。该方法按照SANTE/11945/2015指南在5、10、50和100 ng/g加标水平下进行验证，大多数分析物的回收率在70%至120%之间（相对标准偏差≤20%）。几乎90%的目标农药实现了≤10 ng/g的定量限。在100 ng/g水平下评估了测量不确定度，所有分析物的总体不确定度值均低于22%。
