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建立了高效液相色谱法(HPLC)切换波长检测小麦籽粒中化学杂交剂SQ-1主成分杀雄嗪酸残留的方法。采用改进的QuEChERS方法进行样品前处理,以80%乙醇作为提取溶剂,以PSA(primary secondary amine,N-丙基乙二胺)作为分散净化剂进行分散固相萃取净化。采用Wondasil C18不锈钢柱,以甲醇-0.1%乙酸水溶液(70∶30,V/V)为流动相,流速:1.0 mL/min,切换检测波长程序:0.01～5.00 min,283 nm;5.01～6.30 min,220 nm;6.31～10.00 min,283 nm。结果表明:杀雄嗪酸在0.40～80.00 mg/L范围内线性关系良好,相关系数r=0.9999,在3个添加水平(1.00,8.00和60.00 mg/kg)范围内,平均加标回收率在82.12%～93.20%之间,相对标准偏差为1.1%～1.9%,检出限为0.020 mg/L。
A high performance liquid chromatography (HPLC) switching wavelength detection of wheat grain chemical hybridization agent SQ-1 main component of maleic acid residue method. The samples were pretreated with a modified QuEChERS method, and 80% ethanol was used as the extraction solvent and PSA (primary secondary amine, N-propyl ethylenediamine) was used as the dispersive solid phase extraction and purification. A Wondasil C18 stainless steel column was used with mobile phase of methanol-0.1% acetic acid (70:30, V / V) as the mobile phase at a flow rate of 1.0 mL / min and the detection wavelength was switched between 0.01 and 5.00 min at 283 nm and 5.01-6.30 min , 220 nm; 6.31 ~ 10.00 min, 283 nm. The results showed that there was a good linear relationship between the concentration of androsonic acid in the range of 0.40 ~ 80.00 mg / L, the correlation coefficient was 0.9999. The average recovery was within the range of three addition levels (1.00, 8.00 and 60.00 mg / kg) 82.12% ~ 93.20%, and the relative standard deviations were 1.1% ~ 1.9%. The detection limit was 0.020 mg / L.