固相萃取/超高压液相色谱-质谱/质谱联用技术测定土壤与灌溉水中的矮壮素及缩节胺

Determination of Chlorocholine Chloride and Mepiquat Chloride in Soil and Water Using SPE/UPLC-MS/MS Technique

采用固相萃取技术对土壤和灌溉用水中的矮壮素及缩节胺进行富集处理,并对固相萃取柱的类型和淋洗条件进行优化,采用超高压液相色谱-质谱/质谱联用技术对富集样品进行分离检测。结果表明,灌溉水中矮壮素和缩节胺的加标水平为0.05、0.10、0.20μg/L时,回收率分别为73%～83%和76%～81%,相对标准偏差分别为9.2%～12.4%和7.5%～13.2%,方法的检出限(LOD)为0.02μg/L;土壤中矮壮素和缩节胺的加标水平为0.50、1.00、1.50μg/kg时,回收率分别为76%～91%和79%～90%,相对标准偏差分别为8.2%～11.8%和4.2%～10.7%,方法的检出限为0.125μg/kg。在1.0～50.0μg/L线性范围内,相关系数均大于0.999。采用该方法对新疆焉耆地区的土壤和灌溉水中的矮壮素及缩节胺进行检测,在该地区的土壤及灌溉水中均未检出目标物残留。

A novel method was developed for the determination of chlorocholine chloride（CCC） and mepiquat chloride（MQ） residues in soil and irrigation water based on SPE/HPLC -MS/MS technique. To investigate their enrichment efficiencies to CCC and MQ, 4 kinds of SPE columns were used to pretreat samples, including silica gel column, Cls column and weak cation exchange（WCX） column. The results showed that the highest efficiency was obtained by using WCX column with 5 mL of 10 mmol/L ammonium acetate（containing 0. 1% formic acid） -methanol（1 ： 9） as elution. The separations of analytes were performed on a HILIC column（ 1.7 μm, 2. 1 mm ×50 mm） by a gradient elution using acetonitrile - 10 mmol/L ammonium acetate（containing 0. 1% formic acid） as moblile phase. The mean recoveries of CCC and MQ were in the range of 73%-91% and 76%-90% , respectively, with RSDs of 8.2% - 12.4% and 4. 2% - 13.2% , respectively. The calibration curves of CCC and MQ were linear in the range of 1.0 - 50.0 μg/L with correlation coefficients more than 0. 999. The detection limits of CCC and MQ both were 0. 125 txg/kg for soil samples and 0.02 μg/L for water samples. The method was applied in the real soil and water samples from Karashahr area, Xinjiang, and no CCC and CQ were detected, The method was reliable, robust and sensitive for the determination of CCC and CQ in soil and water samples.