Kim Yool-Ah, Abd El-Aty A M, Rahman Md Musfiqur, Jeong Ji Hoon, Shin Ho-Chul, Wang Jing, Shin SungShik, Shim Jae-Han
Natural Products Chemistry Laboratory, College of Agriculture and Life Sciences, Chonnam National University, Gwangju 500-757, Republic of Korea.
Department of Pharmacology, Faculty of Veterinary Medicine, Cairo University, 12211 Giza, Egypt; Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea.
J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Feb 15;1076:130-138. doi: 10.1016/j.jchromb.2018.01.015.
In the present study, a liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) method with a minimal matrix effect (ME) was developed and validated for simultaneous determination of a diverse range of pesticides (49) in kiwifruit. Samples extracted by the quick, easy, cheap, effective, rugged, and safe (QuEChERS) citrate-buffered method were analyzed either without purification or following purification (with primary secondary amine (PSA) or PSA + graphitized carbon black (GCB)). With the addition of a clean-up step, the suppression of the ME decreased, with a higher number of pesticides determined by the application of PSA + GCB. The method exhibited good linearity with coefficients of determination (R) ≥ 0.9972 and satisfactory recoveries (70-120%) with a relative standard deviations (RSDs) <10%. The limits of quantification (LOQ) were lower than the maximum residue limits (MRLs) set by the Korean Ministry of Food and Drug Safety (MFDS) and the CODEX Alimentarius. The developed method was applied to the real samples and the results indicated that the quantitated levels of all pesticides, except for pyraclostrobin and carbendazim, are lower than the MRLs set by the regulatory authorities. The percentage of the acceptable daily intake was <20%, suggesting that there is no risk associated with the intake of residual pesticides through kiwifruit.
在本研究中,开发并验证了一种具有最小基质效应(ME)的液相色谱-串联质谱(LC-MS/MS)方法,用于同时测定猕猴桃中多种农药(49种)。采用快速、简便、廉价、高效、耐用且安全(QuEChERS)的柠檬酸盐缓冲方法提取的样品,不经净化或经净化(使用伯仲胺(PSA)或PSA + 石墨化炭黑(GCB))后进行分析。通过增加净化步骤,ME的抑制作用降低,使用PSA + GCB可测定更多种类的农药。该方法具有良好的线性,测定系数(R)≥ 0.9972,回收率令人满意(70 - 120%),相对标准偏差(RSD)< 10%。定量限(LOQ)低于韩国食品药品安全部(MFDS)和食品法典委员会设定的最大残留限量(MRL)。将所开发的方法应用于实际样品,结果表明,除吡唑醚菌酯和多菌灵外,所有农药的定量水平均低于监管当局设定的MRL。每日可接受摄入量的百分比< 20%,表明通过食用猕猴桃摄入残留农药不存在风险。