液相色谱-串联质谱法测定土样中太安
LC-MS/MS Determination of Pentaeythritol Tetranitrate in Soil Sample
摘 要
土样经丙酮提取,提取液用液相色谱-串联质谱法进行分析。色谱分离用Agilent SB-C18色谱柱(150 mm×4.6 mm,5 μm)作分离柱,0.05 mmol·L-1氯化铵-甲醇(30+70)溶液为流动相进行洗脱,采用负离子模式电喷雾离子源在多反应监测模式下进行检测。太安的质量浓度在0.25~75 μg·L-1范围内与其峰面积呈线性关系,检出限(3S/N)为0.25 μg·kg-1。以泥土样品为基体,加入3个浓度水平的太安标准做回收试验,测得回收率在92%~97%之间,测定值的相对标准偏差(n=6)在1.1%~2.4%之间。
土样
太安
LC-MS/MS
Soil sample
Pentaeythritol tetranitrate
Abstract
Soil sample was extracted with acetone, and the extract obtained was analyzed by LC-MS/MS. Agilent SB-C18 column (150 mm×4.6 mm, 5 μm) was used as stationary phase. Mixture of 0.05 mmol·L-1 NH4Cl in methanol (30+70) was used as mobile phase and electrospray ionization source with negative ionization mode as well as multiple reaction monitoring mode were used in the MS/MS analysis. Linear relationship between values of peak area and mass concentration of pentaeythritol tetranitrate (PETN) was kept in the range of 0.25-75 μg·L-1, with detection limit (3S/N) of 0.25 μg·kg-1. Tests for recovery were made by addition of standard PETN solution at 3 different concentration levels to samples of clay as matrixes, values of recovery found were in the range of 92%-97%, with values of RSD′s (n=6) in the range of 1.1%-2.4%.
中图分类号 O657.63
所属栏目 工作简报
基金项目 公安部应用创新项目(2010YYCXGAES099)
收稿日期 2011/7/28
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备注张榆梓(1987-),女,山东潍坊人,硕士研究生,主要研究方向为法化学。
引用该论文: ZHANG Yu-zi,ZHOU Hong,SUN Yu-you. LC-MS/MS Determination of Pentaeythritol Tetranitrate in Soil Sample[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(8): 897～899
张榆梓,周红,孙玉友. 液相色谱-串联质谱法测定土样中太安[J]. 理化检验－化学分册, 2012, 48(8): 897～899
被引情况:
【1】孙振文,刘占芳,乔婷,周红,孙玉友,权养科, "激光共聚焦拉曼光谱法检测潜在指纹上的太安",理化检验－化学分册 51, 6-10(2015)
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参考文献
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【15】张敏,孙莉霞,陈智群.BTTN和NG混合物的电喷雾电离质谱研究［J］.含能材料, 2004,12(3):165-167.
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【3】COLLIN O, ZIMMERMANN C, JACKSON G. Fast gas chromatography negative chemical ionization tandem mass spectrometry of explosive compounds using dynamic collision-induced dissociation［J］. International Journal of Mass Spectrometry, 2009,279(10):93-99.
【4】GROOM C, BEAUDET S, HALASZ A. Detection of the cyclic nitramine explosives hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) aoctahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazine (HMX) and their degradation products in soil environments［J］. Journal of Chromatography A, 2001,909(12):53-60.
【5】KAUR G, KUMAR A. SPME-HPLC: A new approach to the analysis of explosives［J］. Journal of Hazardous Materials, 2007,147(5):691-697.
【6】MALIKA A, RAIB P. Development of a new SPME-HPLC-UV method for the analysis of nitro explosives on reverse phase amide column and application to analysis of aqueous samples［J］. Journal of Hazardous Materials, 2009,172(8):1652-1658.
【7】OCHSENBEIN U, ZEH M, BEREST J. Comparing solid phase extraction and direct injection for the analysis of ultra-trace levels of relevant explosives in lake water and tributaries using liquid chromatography-electrospray tandem mass spectrometry［J］. Chemosphere, 2008,72(5):974-980.
【8】MTNG Z, YINION J. Identification of nitrate ester explosives by liquid chromatography-electrospray ionization and atmospheric pressure chemical ionization［J］. Journal of Chromatography A, 2002,798(17):59-68.
【9】XIAOPING P, TIAN K. Method optimization for quantitative analysis ofoctahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) by liquid chromatography electrosprayionization mass spectrometry［J］. Talanta, 2006,70(2):455-459.
【10】VIGNEAU O, XAVIER M. A LC-MS method allowing the analysis of HMX and RDX present at the picogram level in natural aqueous samples without a concentration step［J］. Talanta, 2009,77(9):1609-1613.
【11】杨瑞琴.LC-MS技术及其在炸药方面的应用［J］.中国人民公安大学学报:自然科学版, 2008,56(2):18-20.
【12】任磊,万立华,李隆广,等.乳化炸药爆炸残留物液相色谱-质谱分析［J］.重庆医科大学学报, 2010,35(7):1057-1059.
【13】张敏.RDX和HMX的大气压电喷雾电离质谱分析［J］.火炸药学报, 2006,29(1):77-80.
【14】张敏,齐引绵,高勇.太安的电喷雾电离质谱分析［J］.分析测试学报(增刊), 2008,27(11):258-259.
【15】张敏,孙莉霞,陈智群.BTTN和NG混合物的电喷雾电离质谱研究［J］.含能材料, 2004,12(3):165-167.
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