填充吸附剂微萃取-气相色谱-质谱法定量测定水、流体生物样品中的硝基炸药

P. Bansal, G. Gaurav, N. Nidhi, S. Rani, A. Malik
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引用次数: 0

摘要

建立了一种用填充吸附剂(MEPS)微萃取-气相色谱-质谱联用(GC-MS)技术定量环境和生物样品中2,4,6- tnt及其代谢物和四烷基等12种硝基芳香族化合物的新方法。MEPS使用4mg C18二氧化硅吸附剂插入微体积注射器中进行样品制备。对影响微萃取过程的萃取循环次数、洗涤溶剂、洗涤溶剂用量、洗脱溶剂用量、洗脱溶剂用量、基质pH等参数进行了优化。气相色谱的流动相为氦气。所建立的方法具有良好的测定系数(R2>0.9804),结果令人满意。该方法对所有分析物的提取率均满意(>89.32%),对生物样品的提取率(>87.45%)。检出限为14 ~ 828 pg/mL。该方法具有操作简单、灵敏度高、分辨率高的特点,可用于实际水、流体生物样品中硝基芳香族炸药的定量分析。
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Development of Microextraction by Packed Sorbent - Gas Chromatography-MassSpectrometry Method for Quantification of Nitro-Explosives in Aqueous andFluidic Biological Samples
A new method for quantification of twelve nitroaromatic compounds including 2,4,6-TNT, its metabolites and Tetryl with microextraction by packed sorbent (MEPS), followed by gas chromatography - mass spectrometric (GC-MS) detection in environmental and biological samples is developed. MEPS employ 4 mg of C18 silica sorbent inserted into a micro-volume syringe for sample preparation. Several parameters capable of influencing the microextraction procedure viz., number of extraction cycles, washing solvent, volume of washing solvent, elution solvent, elution solvent volume and pH of matrix etc., were optimized. Helium gas was used as mobile phase during GC operation. The developed method produced satisfactory results with excellent values of coefficient of determination (R2>0.9804) within the established calibration range. The extraction yields were satisfactory for all analytes (>89.32%) for aqueous samples and (>87.45%) for biological samples. The limits of detection values lie in the range 14 - 828 pg/mL. Due to procedural simplicity, high sensitivity and efficient resolution of all analytes, the developed method was applied successfully for quantification of nitro aromatic explosives in real aqueous and fluidic biological samples.
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