Nanita Sergio C, Pentz Anne M, Bramble Frederick Q
DuPont Crop Protection, Stine-Haskell Research Center, 1090 Elkton Road, Newark, Delaware 19714, USA.
Anal Chem. 2009 Apr 15;81(8):3134-42. doi: 10.1021/ac900226w.
The use of automated flow injection with MS/MS detection for fast quantitation of agrochemicals in food and water samples was demonstrated in this study. Active ingredients from the sulfonylurea herbicide and carbamate insecticide classes were selected as model systems. Samples were prepared using typical procedures from residue methods, placed in an autosampler, and injected directly into a triple quadrupole instrument without chromatographic separation. The technique allows data acquisition in 15 s per injection, with samples being injected every 65 s, representing a significant improvement from the 15-30 min needed in typical HPLC/MS/MS methods. The availability of HPLC systems is an advantage since they can be used in flow-injection mode (bypassing the column compartment). Adequate accuracy, linearity, and precision (R(2) > 0.99 and RSD < 20%) were obtained using external standards prepared in each control matrix. The limit of quantitation (LOQ) achieved for all analytes was 0.01 mg/kg in food samples and 0.1 ng/mL in water; while limits of detection (LOD) were estimated to be about 0.003 mg/kg and 0.03 ng/mL in food and water, respectively. The advantages and limitations of flow injection MS/MS for ultratrace-level quantitative analysis in complex matrixes are discussed.
本研究展示了使用自动流动注射与串联质谱检测技术对食品和水样中的农用化学品进行快速定量分析。选择磺酰脲类除草剂和氨基甲酸酯类杀虫剂的活性成分作为模型体系。样品采用残留分析方法的典型程序进行制备，置于自动进样器中，直接注入三重四极杆仪器，无需色谱分离。该技术每次进样可在15秒内完成数据采集，每65秒进样一次，与典型的高效液相色谱/串联质谱方法所需的15 - 30分钟相比有显著改进。高效液相色谱系统的可用性是一个优势，因为它们可以用于流动注射模式（绕过柱箱）。使用在每个对照基质中制备的外标法获得了足够的准确度、线性和精密度（R(2) > 0.99且相对标准偏差 < 20%）。食品样品中所有分析物的定量限（LOQ）为0.01 mg/kg，水样中为0.1 ng/mL；而食品和水中的检测限（LOD）分别估计约为0.003 mg/kg和0.03 ng/mL。讨论了流动注射串联质谱在复杂基质中超痕量定量分析的优缺点。
