Department of Fisheries and Wildlife, Michigan State University, East Lansing, Michigan 48824, United States.
Environ Sci Technol. 2011 Aug 1;45(15):6437-43. doi: 10.1021/es200416f. Epub 2011 Jul 13.
We developed an assay for measuring 7α,12α,24-trihydroxy-5a-cholan-3-one-24-sulfate (3kPZS), a mating pheromone released by male sea lampreys (Petromyzon marinus), at low picomolar concentrations in natural waters to assess the presence of invasive populations. 3kPZS was extracted from streamwater at a rate of recovery up to 90% using a single cation-exchange and reversed-phase mixed-mode cartridge, along with [(2)H(5)]3kPZS as an internal standard, and quantified using ultrahigh performance liquid chromatography-tandem mass spectrometry. The limit of detection was below 0.1 ng L(-1) (210 fM), which was the lowest concentration tested. Intra- and interday coefficients of variation were between 0.3-11.6% and 4.8-9.8%, respectively, at 1 ng 3kPZS L(-1) and 5 ng 3kPZS L(-1). This assay was validated by repeat measurements of water samples from a stream spiked with synthesized 3kPZS to reach 4.74 ng L(-1) or 0.24 ng L(-1). We further verified the utility of this assay to detect spawning populations of lampreys; in the seven tributaries to the Laurentian Great Lakes sampled, 3kPZS concentrations were found to range between 0.15 and 2.85 ng L(-1) during the spawning season in known sea lamprey infested segments and were not detectable in uninfested segments. The 3kPZS assay may be useful for the integrated management of sea lamprey, an invasive species in the Great Lakes where pheromone-based control and assessment techniques are desired.
我们开发了一种测定方法，可用于测量低皮摩尔浓度下天然水中的 7α,12α,24-三羟基-5α-胆烷-3-酮-24-硫酸盐（3kPZS），这是雄性海七鳃鳗（Petromyzon marinus）释放的交配信息素，以评估入侵种群的存在。3kPZS 采用单阳离子交换和反相混合模式柱以回收率高达 90%的方式从溪流水中提取，同时使用 [(2)H(5)]3kPZS 作为内标，并采用超高效液相色谱-串联质谱进行定量。检测限低于 0.1ng L(-1)（210fM），这是测试的最低浓度。在 1ng 3kPZS L(-1)和 5ng 3kPZS L(-1)时，内标和日间变异系数分别在 0.3-11.6%和 4.8-9.8%之间。该测定方法通过对合成 3kPZS 加入溪流水样进行重复测量进行了验证，达到 4.74ng L(-1)或 0.24ng L(-1)。我们进一步验证了该测定方法检测七鳃鳗产卵种群的效用；在所采样的七大流入湖的支流中，在已知有海七鳃鳗出没的产卵季节，3kPZS 浓度在 0.15 和 2.85ng L(-1)之间，而在无七鳃鳗出没的地段则无法检测到。该 3kPZS 测定方法可能对大湖地区的海七鳃鳗（一种入侵物种）的综合管理有用，大湖地区需要基于信息素的控制和评估技术。
