Skarping G, Dalene M D, Tinnerberg H
Department of Occupational and Environmental Medicine, University Hospital, Lund, Sweden.
Analyst. 1994 Sep;119(9):2051-5. doi: 10.1039/an9941902051.
Hexamethylene-1,6-diamine (HDA) and isophoronediamine (IPDA) in hydrolysed human urine were studied as their perfluorofatty anhydride derivatives. Liquid chromatography and mass spectrometry with thermospray ionization were used. For quantitative analysis, the negative ions monitored were the m/z = 407 and 461, corresponding to the (M-1)- ions of the HDA-pentafluoropropionic anhydride (HDA-PFPA) and the IPDA-PFPA derivatives, respectively, and the m/z = 411 ions of the tetradeuterium-labelled HDA-PFPA (internal standard). Human urine was spiked with HDA and IPDA to six different concentrations in the range 2.5-20 micrograms l-1. Tetradeuterated HDA was used as the internal standard for the determination of both HDA and IPDA. The linear calibration curves obtained passed virtually through the origin, and the correlation coefficients were 0.998 for HDA and 0.973 for IPDA. The over-all precision for human urine spiked to a concentration of 5 micrograms l-1 of HDA and 25 micrograms l-1 of IPDA was found to be 5 and 14% (n = 5), respectively. The m/z = (M-1)- fragments, defined as twice the signal-to-noise ratio, were at the 0.5-1 pg level for the HDA and IPDA derivatives. The method presented made it possible to perform about 400 chromatographic runs during 24 h.
对水解人尿中的六亚甲基 -1,6 -二胺(HDA)和异佛尔酮二胺(IPDA)作为其全氟脂肪酸酐衍生物进行了研究。采用了带热喷雾电离的液相色谱和质谱联用技术。进行定量分析时,监测的负离子分别为质荷比(m/z = 407)和(461),它们分别对应于HDA - 五氟丙酸酐(HDA - PFPA)和IPDA - PFPA衍生物的((M - 1)^-)离子,以及氘代十四烷标记的HDA - PFPA(内标)的质荷比(m/z = 411)离子。向人尿中加入HDA和IPDA,使其浓度在(2.5 - 20)微克/升范围内达到六种不同水平。氘代HDA用作测定HDA和IPDA的内标。得到的线性校准曲线几乎都通过原点,HDA的相关系数为(0.998),IPDA的相关系数为(0.973)。对于添加了浓度为(5)微克/升的HDA和(25)微克/升的IPDA的人尿,总体精密度分别为(5%)和(14%)((n = 5))。对于HDA和IPDA衍生物,定义为信噪比两倍的(m/z = (M - 1)^-)碎片在(0.5 - 1)皮克水平。所提出的方法使得在(24)小时内能够进行约(400)次色谱分析。