除草剂2，4-D丁酯的GC/MS检测及其在中毒患者诊治中的应用

The applicabion of 2,4-D butyl ester in the blood of acute poisoning patients by gas chromatograpy-mass spectrometry(GC/MS)

目的建立除草剂2,4-D丁酯的气相色谱一质谱(GC/MS)检测方法,用于临床中毒患者的检测。方法以乙酸乙酯提取血液中2,4D丁酯,采用GC/MS检测。定性采用全扫描法(SCAN),定量采用选择离子法(SIM),离子选择m/z 175、185、276。结果2,4-D丁酯在10～1500 ng/ml成线性,方程为Y=10.565X-1203.5,R=0.9941,标加1000 ng/ml浓度的2,4-D丁酯于血液,平均回收率为94.6%,RSD=7.1%;2,4-D丁酯最低检出浓度为3 ng/ml(SIM),信噪比S/N=3;日内精密度RSD为4.1%,日间精密度RSD为5.8%。结论所建方法灵敏、快速、线性范围好,可用于2,4-D丁酯中毒患者的检测。

Objective To establish a method for the determination of 2, 4-D butyl ester in blood of acute poisoning patients by gas chromatograpy-mass spectrometry （GC/MS）. Method The 2, 4-D butyl ester in blood was extracted with acetic ether, and separated the acetic ether from the blood by warming the cetic ether with water at 60℃ and blowing with nitrogen gas to 100μl for detection of 2, 4-D butyl ester by GC/MS. The standard curve, the detection limit, and the repeatability of 2, 4-D bytyl ester were established. Results The results showed that the linear calibration curve of 2, 4-D butyl ester was Y= 10.565X - 1203.5, R = 0.9941, and the range of concentration was 10-1500 ng/ml. The extraction yield of acetic ether for 2, 4-D butyl ester in blood was 94.6%, RSD = 7.1%, n = 6, and it＇s an ideal solvent for 2, 4-D butyl ester extraction. The lowest detection limit was 3 ng/ml （SIM： m/z175, 185, 276; S/N = 3）. The RSD of precision within a day was 4.1%. The RSD of was precision between days was 5.8%. Conclusions The extraction and analysis method is suitable and can be applied to the diagnosis of the acute poisoning patient of 2, 4-D butyl ester.