Centers for Disease Control and Prevention, 4770 Buford Highway, Atlanta, GA 30341, USA.
J Anal Toxicol. 2010 Apr;34(3):122-8. doi: 10.1093/jat/34.3.122.
A high-throughput method has been developed for determining Lewisite [dichloro(2-chlorovinyl)arsine] exposure by measuring the urine metabolite 2-chlorovinylarsonous acid (CVAA) and the oxidized metabolite 2-chlorovinylarsonic acid (CVAOA). The rapid sample preparation included a simple dilution of 400 microL of urine with 40 microL of water and 1 mL of buffer containing an internal standard and brief centrifugation prior to analysis by high-performance liquid chromatography-inductively coupled plasma-mass spectrometry (ICP-MS). CVAOA and CVAA were eluted isocratically with retention factors of approximately 3.0 and 4.2, respectively, from a reversed-phase polar embedded column with a cycle time of 5 min per sample. The dynamic reaction cell, typically used to remove polyatomic isobaric interferences, was not required for ICP-MS analysis because of the resolution of chloride from arsenical peaks of interest. This method was used to detect CVAA and CVAOA in the urine of a rat administered Lewisite up to 24 h after exposure. The method demonstrated linearity over at least three orders of magnitude and had a method detection limit of 1.3 microg/L as CVAA (1.4 microg/L CVAOA). The relative standard deviations for quality control samples ranged from 3 to 6%. The method was sensitive and selective with no false positives in 100 different urine samples collected from individuals with no known exposure to Lewisite. Ninety-six samples could be analyzed in an 8-h day.
已开发出一种高通量方法，通过测量尿液代谢物 2-氯乙烯基胂酸（CVAA）和氧化代谢物 2-氯乙烯基胂酸（CVAOA）来测定路易氏剂（二氯（2-氯乙烯基）胂）暴露。快速的样品制备包括将 400μL 尿液用 40μL 水和 1mL 含内标物的缓冲液简单稀释，然后在分析前短暂离心，采用高效液相色谱-电感耦合等离子体质谱法（ICP-MS）进行分析。CVAOA 和 CVAA 采用反相极性嵌入柱进行等度洗脱，保留因子分别约为 3.0 和 4.2，每个样品的循环时间为 5min。由于氯化物与感兴趣的砷化峰分离，因此不需要动态反应池来消除多原子同量异位干扰，即可进行 ICP-MS 分析。该方法用于检测暴露于路易氏剂后 24 小时内大鼠尿液中的 CVAA 和 CVAOA。该方法在至少三个数量级范围内表现出线性，CVAA 的方法检测限为 1.3μg/L（CVAOA 为 1.4μg/L）。质控样品的相对标准偏差范围为 3%至 6%。该方法灵敏且具有选择性，在收集自无已知路易氏剂暴露个体的 100 份不同尿液样本中未出现假阳性。每天可分析 96 个样品。
