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高氯酸盐作为一类广泛分布的环境污染物，其在地表水中的含量水平对生态系统及人体健康存在潜在影响。通过建立高效液相色谱-串联三重四极杆质谱(HPLC-MS/MS)同位素稀释内标法测定地表水中的高氯酸盐，并系统优化了色谱分离参数(流动相种类、浓度、柱温)与质谱离子化参数。结果表明，该方法在0.20～20μg/L范围内呈现良好线性关系(相关系数0.999 92)，高氯酸盐检出限为0.05μg/L。标准溶液及有证标准物质测定结果的相对标准偏差为0.18%～7.7%(n=6)，相对误差为-3%～1.1%(n=6)。地下水、地表水、生活污水及工业废水等实际样品的加标回收率为86.9%～99.9%(n=6)。应用该方法对长江流域四川段地表水进行监测，高氯酸盐检出率达97%，平均浓度为1.88μg/L。
Abstract：Perchlorate,as a class of widely distributed environmental pollutants,poses potential risks to ecosystems and human health due to its levels in surface water. An isotope dilution internal standard method usinghigh-performance liquid chromatography-tandem triple quadrupole mass spectrometry( HPLC-MS/MS)was established for the determination of perchlorate in surface water. Chromatographic separation parameters( mobile phase type,concentration,and column temperature) and mass spectrometric ionization parameters were systematically optimized. Results indicated that the method exhibited a good linear relationship within the range of 0. 20-20 μg/L( correlation coefficient: 0. 99992),with a perchlorate detection limit of 0. 05 μg/L. The relative standard deviations( RSDs) for standard solutions and certified reference materials ranged between0. 18% and 7. 7%( n = 6),and the relative errors( REs) ranged from-3. 0% to 1. 1%( n = 6). Spike recovery rates for actual samples,including groundwater,surface water,domestic wastewater,and industrial wastewater,ranged from 86. 9% to 99. 9%( n = 6). Application of this method to monitor surface water in the Sichuan section of the Yangtze River Basin revealed a perchlorate detection rate of 97%,with an average concentration of 1. 88 μg/L.
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基本信息:
DOI：10.14034/j.cnki.schj.2026.06.017
中图分类号:X832;O657.63
引用信息:
[1]张翔龙,周舟,王若男,等.HPLC-MS/MS法测定地表水中的高氯酸盐[J].四川环境,2026,45(01):141-149.DOI:10.14034/j.cnki.schj.2026.06.017.