Cheng Zhipeng, Dong Fengshou, Xu Jun, Liu Xingang, Wu Xiaohu, Chen Zenglong, Pan Xinglu, Zheng Yongquan
State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing, 100193, PR China.
State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing, 100193, PR China.
J Chromatogr A. 2016 Feb 26;1435:115-24. doi: 10.1016/j.chroma.2016.01.025. Epub 2016 Jan 15.
In this study, the application of atmospheric pressure gas chromatography quadrupole-time-of-flight mass spectrometry (APGC-QTOF-MS) has been investigated for simultaneous determination of fifteen organochlorine pesticides in soil and water. Soft ionization of atmospheric pressure gas chromatography was evaluated by comparing with traditional more energetic electron impact ionization (EI). APGC-QTOF-MS showed a sensitivity enhancement by approximately 7-305 times. The QuEChERs (Quick, Easy, Cheap, Effective, Rugged, and Safe) method was used to pretreat the soil samples and solid phase extraction (SPE) cleanup was used for water samples. Precision, accuracy and stability experiments were undertaken to evaluate the feasibility of the method. The results showed that the mean recoveries for all the pesticides from the soil samples were 70.3-118.9% with 0.4-18.3% intra-day relative standard deviations (RSD) and 1.0-15.6% inter-day RSD at 10, 50 and 500 μg/L levels, while the mean recoveries of water samples were 70.0-118.0% with 1.1-17.8% intra-day RSD and 0.5-12.2% inter-day RSD at 0.1, 0.5 and 1.0 μg/L levels. Excellent linearity (0.9931 ≦ r(2)≤ 0.9999) was obtained for each pesticides in the soil and water matrix calibration curves within the range of 0.01-1.0mg/L. The limits of detection (LOD) for each of the 15 pesticides was less than 3.00 μg/L, while the limit of quantification (LOQ) was less than 9.99 μg/L in soil and water. Furthermore, the developed method was successfully applied to monitor the targeted pesticides in real soil and water samples.
在本研究中,对大气压气相色谱 - 四极杆飞行时间质谱(APGC - QTOF - MS)用于同时测定土壤和水中15种有机氯农药的应用进行了研究。通过与传统的能量更高的电子轰击电离(EI)进行比较,评估了大气压气相色谱的软电离。APGC - QTOF - MS的灵敏度提高了约7 - 305倍。采用QuEChERs(快速、简便、廉价、有效、耐用且安全)方法对土壤样品进行预处理,对水样采用固相萃取(SPE)净化。进行了精密度、准确度和稳定性实验以评估该方法的可行性。结果表明,在10、50和500μg/L水平下,土壤样品中所有农药的平均回收率为70.3 - 118.9%,日内相对标准偏差(RSD)为0.4 - 18.3%,日间RSD为1.0 - 15.6%;而在0.1、0.5和1.0μg/L水平下,水样的平均回收率为70.0 - 118.0%,日内RSD为1.1 - 17.8%,日间RSD为0.5 - 12.2%。在0.01 - 1.0mg/L范围内,土壤和水基质校准曲线中每种农药均获得了良好的线性(0.9931≦r²≤0.9999)。15种农药中每种农药在土壤和水中的检测限(LOD)均小于3.00μg/L,定量限(LOQ)均小于9.99μg/L。此外,所建立的方法成功应用于监测实际土壤和水样中的目标农药。