微波萃取_气相色谱_气相色谱_质谱法测定土壤中18种有机氯农药.pdfVIP

2010 4 Vol. 29, No. 2 April 2010 ROCK AND M INERAL ANALYSIS 118~ 122 : 02 4 3 7( 2010) 02 0118 0 微波萃取- 气相色谱 /气相色谱- 质谱法测定土壤中 18种有机氯农药 李庆霞, 刘亚轩, 陈卫明, 张 勤 (, 06 000) : 采用微波萃取- F lorisil固相萃取柱净化分离气相色谱和气相色谱 - 质谱相结合 方法测定土壤 中 痕量半挥发性有机氯农药优化了微波萃取和固相萃取柱净化条件, 在最优条件下 18种有机氯农药 ( - HCH- HCH - HCH!- HCH七氯艾氏剂环氧七氯硫丹p, p - DDE狄氏剂异狄氏剂硫 丹!p, p - DDDo, p - DDT异狄氏剂醛硫丹硫酸酯p, p - DDT甲氧滴滴涕) 回收率在 89. 6% ~ 114. 22% 对气相色谱和气相色谱 -质谱法 仪器检出限回收率精密度和方法检出限进行对比, 确定 了采用气相色谱- 质谱定性和气相色谱定量相结合 方法, 测定实际土壤样品中 有机氯农药, 使得定性 和定量 准确度都得到提高 : 微波萃取; 气相色谱法; 气相色谱- 质谱法; 有机氯农药; 土壤 : O6 7. 63; S482. 32; S1 1. 93 : A Determination of 18 OrganochlorinePesticides in SoilsbyGas Chromatography andGasChromatographyMass Spectrometry withM icrowaveassisted Extraction LI Q ing x ia, LI U Yaxuan, CH EN W eim ing, ZHAN G Q in ( Centra l Labo ra tory, Institute o f Geophys ica l Geochem ica l Exp lora tion, Ch inese A cademy o f Geo log ica l Sc ei nces, Lang fang 06 000, C h ina) Abstract: A samp le pretreatmentmethod ofm icrow aveassisted extractionFlorisil solid phase extraction cleanup for gas chromatographic ( GC) and gas chromatographymass spectrometric ( GCM S) determ ination of the trace sem ivolatile organochlorine pesticides in soilsw as developed. Them icrow aveassisted extraction and F lorisil solid phase extraction conditions w ere optmi ized. Under the optmi um cond ition, the recoveries of 18 organochlorine pesticides ( HCH, HCH, HCH, !HCH, heptachlor, aldrin, heptachlor epoxide, endosu lfan, p, p DDE, dieldrin, endrin, endosu lfan !, p, p DDD, o, p DDT, endrin aldehyde, endosulfan sulfate, p, p DDT, methoxychlor) w ere 89. 6% ~ 114. 22%. The instrument detection lmi it, recovery, precision and detection lmi it ofmethodw ere compared bewt een GC and GCMS. Based on the combin