皮革中多菌灵等三种防霉剂的检测方法研究

Study on Determination of Carbendazim,Chlorothalonil and Thiophanate-methy1 in Leather

应用固相萃取及高效液相色谱技术，建立了同时测定皮革中多菌灵、百菌清和甲基托布津含量的方法。皮革样品经乙腈超声提取后，由弗罗里硅土固相萃取小柱净化，以Agilent Eclipse Plus C18（4.6×250 mm，5μm）色谱柱为分析柱，乙酸铵水溶液一甲醇为流动相，线性梯度淋洗，紫外二极管矩阵检测器检测，波长为240或270 nm。结果表明，多菌灵、百菌清和甲基托布津在0.5～15.0 mg·L-1范围内有良好的线性关系，方法的定量下限（S/N=10）分别为0.06、0.8、0.5 mg·kg-1，加标回收率为90.2％～97.7％，变异系数（CV）不大于7.9％。

A solid phase extraction （SPE）coupled to high performance liquid chromatographic （HPLC） method was developed for determination of carbendazim , chlorothalonil and thiophanate-methyl in Leather. The sample was extracted with acetonitrile by ultrasound-assisted extraction,and purified by florisil SPE column. The detection of thiophanate-methyl, chlorothalonil and carbendazim was carried out by HPLC using Agilent Eclipse Plus C18 （4.6 ×250 mm,5μm） column as separation column,10 mmol·L-1 ammonium acetate solution-methanol as mobile phase. The UV detecting wavelength was set at 240nm or 270nm. The result indicated that the calibration curves of carbendazim, chlorothalonil and thiophanate-methyl were linear in the range of 0.5-15.0 mg·L-1 with limits of quantification （LOQs） of 0.06, 0.8, 0.5 mg·kg-1,respectively.The spiked recoveries of carbendazim, chlorothalonil and thiophanate-methyl were in the range of 90.2%-97.7% with CV （n=6） not more than 7.9%.