Article ID | Journal | Published Year | Pages | File Type |
---|---|---|---|---|
7615853 | Journal of Chromatography B | 2017 | 20 Pages |
Abstract
A simple and rapid gas chromatography-flame photometric detection (GC-FPD) method was developed for the determination of 12 organophosphorus pesticides (OPPs) in Salvia miltiorrhizae by using ultrasonication assisted one-step extraction (USAE) without any clean-up steps. Some crucial parameters such as type of extraction solvent were optimized to improve the method performance for trace analysis. Any clean-up steps were negligent as no interferences were detected in the GC-FPD chromatograms for sensitive detection. Under the optimized conditions, limits of detection (LODs) and quantitation (LOQs) for all pesticides were in the range of 0.001-0.002Â mg/kg and 0.002-0.01Â mg/kg and 0.002-0.01Â mg/kg, respectively, which were all below the regulatory maximum residue limits suggested. RSDs for method precision (intra- and inter-day variations) were lower than 6.8% in approval with international regulations. Average recovery rates for all pesticides at three fortification levels (0.5, 1.0 and 5.0Â mg/kg) were in the range of 71.2-101.0% with relative standard deviations (RSDs) <13%. The developed method was evaluated for its feasibility in the simultaneous pre-concentration and determination of 12 OPPs in 32 batches of real S. miltiorrhizae samples. Only one pesticide (dimethoate) out of the 12 targets was simultaneously detected in four samples at concentrations of 0.016-0.02Â mg/kg. Dichlorvos and omethoate were found in the same sample from Sichuan province at 0.004 and 0.027Â mg/kg, respectively. Malathion and monocrotophos were determined in the other two samples at 0.014 and 0.028Â mg/kg, respectively. All the positive samples were confirmed by LC-MS/MS. The simple, reliable and rapid USAE-GC-FPD method with many advantages over traditional techniques would be preferred for trace analysis of multiple pesticides in more complex matrices.
Keywords
Related Topics
Physical Sciences and Engineering
Chemistry
Analytical Chemistry
Authors
Shanshan Zhang, Xiaofei Liu, Jia'an Qin, Meihua Yang, Hongzheng Zhao, Yong Wang, Weiying Guo, Zhijie Ma, Weijun Kong,