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建立了土壤中痕量二苯羟乙酸-3-喹咛环酯(BZ)的液相色谱-四极杆飞行时间串联质谱检测方法。BZ含量在10~400 ng/m L范围内呈良好线性关系,相关系数为0.9992,仪器定量限为5 ng/m L;在ESS-1标准土壤中的方法检出限为6.5 ng/g,在花园土中的方法检出限为6.5 ng/g;在沙土中的方法检出限为7.4 ng/g。对上述3种土壤中的BZ进行不同水平的加标回收率实验,得到方法的回收率为71%~97%,相对标准偏差(n=3)为1.3%~10%。方法已用于实际样品的检测。通过对BZ电喷雾二级质谱主要裂解途径的研究,明确了特征碎片离子的结构。
A liquid chromatographic-quadrupole time of flight tandem mass spectrometry (MS-MS / MS) method was developed for the determination of trace amount of benzodiazepin (BZ) in soil. The linear range of BZ was 10-400 ng / mL, with a correlation coefficient of 0.9992 and a limit of quantification of 5 ng / mL. The detection limit was 6.5 ng / g in ESS-1 standard soils, The method detection limit in garden soil is 6.5 ng / g; the detection limit in soil is 7.4 ng / g. The recoveries of BZ in the three soils were varied from 71% to 97% with relative standard deviations (n = 3) of 1.3% -10%. The method has been used for the detection of actual samples. Through the study of the main cleavage pathway of BZ electrospray ionization mass spectrometry, the structure of the characteristic fragment ions was clarified.