Baker Samuel E, Olsson Anders O, Barr Dana B
Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, 4771 Buford Highway, N.E., Atlanta, Georgia 30341, USA.
Arch Environ Contam Toxicol. 2004 Apr;46(3):281-8. doi: 10.1007/s00244-003-3044-3.
This paper describes a method for measuring cis- and trans-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropane-1-carboxylic acids (cis-DCCA and trans-DCCA), cis-3-(2,2-dibromovinyl)-2,2-dimethylcyclopropane-1-carboxylic acid (DBCA), 3-phenoxybenzoic acid (3PBA), and 4-fluoro-3-phenoxybenzoic acid (4F3PBA) in human urine. These compounds are considered to be reliable biomarkers of exposure for many pyrethroid insecticides used in the United States. In this method, stable isotopically labeled analogues of trans-DCCA and 3PBA were spiked into urine as internal standards. After solid-phase extraction, the extracts were analyzed by high-performance liquid chromatography coupled with tandem mass spectrometry using turbo ion-spray atmospheric pressure ionization. The limits of detection (LODs) ranged from 0.1 to 0.5 microg/L. Within-day relative standard deviations ranged from 1.8 to 13% and between-day relative standard deviations ranged from 0.5 to 18%. Absolute analyte recoveries ranged from 72 to 93%. Chromatographic retention times were less than 8 min. This method was used to measure urinary concentrations of these metabolites in persons with no known exposure to pyrethroids and some with suspected residential exposure. Metabolites of synthetic pyrethroids were detected in 74% of the samples analyzed. cis-DCCA, trans-DCCA, DBCA, 4F3PBA, and 3PBA were detected in 36, 50, 3, 9, and 64% of the samples analyzed, respectively.
本文介绍了一种测定人尿中顺式和反式3-(2,2-二氯乙烯基)-2,2-二甲基环丙烷-1-羧酸(顺式DCCA和反式DCCA)、顺式3-(2,2-二溴乙烯基)-2,2-二甲基环丙烷-1-羧酸(DBCA)、3-苯氧基苯甲酸(3PBA)和4-氟-3-苯氧基苯甲酸(4F3PBA)的方法。这些化合物被认为是美国使用的许多拟除虫菊酯类杀虫剂暴露的可靠生物标志物。在该方法中,将反式DCCA和3PBA的稳定同位素标记类似物作为内标加入尿液中。固相萃取后,提取物通过高效液相色谱-串联质谱联用,采用涡轮离子喷雾大气压电离进行分析。检测限(LOD)范围为0.1至0.5μg/L。日内相对标准偏差范围为1.8%至13%,日间相对标准偏差范围为0.5%至18%。分析物的绝对回收率范围为72%至93%。色谱保留时间小于8分钟。该方法用于测量无已知拟除虫菊酯暴露者和一些疑似居住暴露者尿液中这些代谢物的浓度。在分析的74%的样本中检测到了合成拟除虫菊酯的代谢物。在分析的样本中,分别有36%、50%、3%、9%和64%检测到了顺式DCCA、反式DCCA、DBCA、4F3PBA和3PBA。