Malik Ashok Kumar, Rai Parmod Kumar
Department of Chemistry, Punjabi University, Patiala, Punjab, India.
J Sep Sci. 2008 Jul;31(12):2173-81. doi: 10.1002/jssc.200800001.
A simple and sensitive method has been developed using preconcentration technique solid phase microextraction (SPME) and analytical technique HPLC-UV for the determination of octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) and hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) from the environmental samples. Aqueous solution of anionic surfactant SDS was used for the extraction of both nitramine high explosives, viz., HMX and RDX from soil samples which were subsequently sorbed on SPME fiber. The static desorption was carried out in the desorption chamber of the SPME-HPLC interface in the presence of mobile phase ACN/methanol/water (30:35:35) and the subsequent chromatographic analysis at a flow rate of 0.5 mL/min and detection at 230 nm. For this purpose, a C(18), 5 microm RP analytical column was used as a separation medium in this method. Several parameters relating to SPME, e.g., adsorption/desorption time, concentration of salt, stirring rate, etc., were optimized. The method was linear over the range of 20-400 ng/mL for HMX and RDX standards in the presence of surfactant in aqueous phase, respectively. The correlation coefficient (R(2)) for HMX and RDX are 0.9998 and 0.9982, respectively. With SPME, the detection limits (S/N = 3) in ng/mL are 0.05 and 0.1 for HMX and RDX, respectively in the presence of the SDS surfactant. The developed method has been applied successfully to the analysis of real environmental samples like bore well water, river water, and ground alluvial soil.
已开发出一种简单且灵敏的方法，该方法采用预浓缩技术固相微萃取（SPME）和分析技术高效液相色谱 - 紫外检测法（HPLC - UV），用于测定环境样品中的八氢 - 1,3,5,7 - 四硝基 - 1,3,5,7 - 四氮杂环辛烷（HMX）和六氢 - 1,3,5 - 三硝基 - 1,3,5 - 三嗪（RDX）。使用阴离子表面活性剂十二烷基硫酸钠（SDS）的水溶液从土壤样品中萃取硝胺类高能炸药HMX和RDX，随后它们被吸附在SPME纤维上。在流动相乙腈/甲醇/水（30:35:35）存在的情况下，在SPME - HPLC接口的解吸室中进行静态解吸，随后以0.5 mL/min的流速进行色谱分析，并在230 nm处进行检测。为此，在该方法中使用C(18)、5微米的反相分析柱作为分离介质。对与SPME相关的几个参数，如吸附/解吸时间、盐浓度、搅拌速率等进行了优化。在水相中存在表面活性剂的情况下，该方法对HMX和RDX标准品的线性范围分别为20 - 400 ng/mL。HMX和RDX的相关系数（R(2)）分别为0.9998和0.9982。使用SPME时，在SDS表面活性剂存在的情况下，HMX和RDX的检测限（S/N = 3）分别为0.05 ng/mL和0.1 ng/mL。所开发的方法已成功应用于实际环境样品的分析，如井水、河水和地表冲积土。
