Gui Wen-jun, Tian Jie, Tian Chun-xia, Li Shu-ying, Ma You-ning, Zhu Guo-nian
Institute of Pesticide and Environmental Toxicology, Zhejiang University, 268 Kaixuan Road, Hangzhou 310029, Zhejiang, China.
Zhenjiang Institute of Termite Control, 65 Yunhe Road, Zhengjiang 212003, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Dec 1;972:102-10. doi: 10.1016/j.jchromb.2014.09.022. Epub 2014 Sep 28.
A reliable and rapid method has been optimized to determine the residue of amicarthiazol in soil and environmental water samples. After extraction and evaporation, the extraction was carried out with solid phase extraction (SPE) cleanup using HLB cartridge (only soil samples) and for the quantitative determination by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The resulting residues of amicarthiazol were analyzed by a gradient separation performed on a UPLC system with a C18 column, methanol and water containing 0.1% (v v(-1)) formic acid as the mobile phase in the mode of electrospray positive ionization (ESI(+)) and multiple reaction monitoring (MRM). Results showed that the recoveries for spiked samples were 74.4-97.1% and 72.1-109.9% for soil and water, respectively, with the relative standard deviation (RSD) less than 10.2% when fortified at 10, 100 and 1000μgL(-1). The limits of detection (LODs) and the limits of quantification (LOQs) for matrix matched standards ranged from 0.073-0.425μgL(-1) and 0.243-1.42μgL(-1). The intra-day precision (n=5) and the inter-day precision over 10 days (n=10) for the amicarthiazol in soils and water samples spiked at 100μgL(-1) was 7.9% and 15.9%, respectively. Results indicated that the developed method could be a helpful tool for the controlling and monitoring of the risks posed by amicarthiazol to human health and environment safety.
已优化出一种可靠且快速的方法来测定土壤和环境水样中灭螨猛的残留量。萃取并蒸发后，采用HLB柱进行固相萃取（SPE）净化（仅针对土壤样品），并通过超高效液相色谱 - 串联质谱法（UPLC - MS/MS）进行定量测定。灭螨猛的残留量通过在配备C18柱的UPLC系统上进行梯度分离进行分析，以含0.1%（v v⁻¹）甲酸的甲醇和水作为流动相，采用电喷雾正离子化（ESI(+)）和多反应监测（MRM）模式。结果表明，加标样品在土壤和水中的回收率分别为74.4 - 97.1%和72.1 - 109.9%，在10、100和1000μg L⁻¹加标水平下，相对标准偏差（RSD）小于10.2%。基质匹配标准品的检测限（LOD）和定量限（LOQ）范围分别为0.073 - 0.425μg L⁻¹和0.243 - 1.42μg L⁻¹。在100μg L⁻¹加标的土壤和水样中，灭螨猛的日内精密度（n = 5）和10天内的日间精密度（n = 10）分别为7.9%和15.9%。结果表明，所建立的方法可为控制和监测灭螨猛对人类健康和环境安全造成的风险提供有用工具。
