Wu W S, Szklar R S, Smith R
Occupational Health Laboratory, Ontario Ministry of Labour, Weston, Ontario, Canada.
Analyst. 1996 Mar;121(3):321-4. doi: 10.1039/an9962100321.
An analytical method for monitoring 4,4'-methylenebis(2-chloroaniline) (MOCA) in urine was developed. The MOCA extract from a urine sample was derivatized with pentafluoropropionic anhydride and subsequently cleaned-up via TLC before being analysed by a gas chromatograph equipped with an electron capture detector. Heptafluorobutyric anhydride derivatized MOCA was used as the internal standard during quantification. The method showed that the analytical interferences are effectively minimized by using the TLC technique for sample clean-up. Recoveries of spiked MOCA in urine at levels of 7.5, 22 and 62.5 micrograms dm-3 were all over 90% with the limit of detection determined to be 1 microgram dm-3. Confirmation of MOCA in a urine sample was performed by using a gas chromatograph mass spectrometer in negative-ion chemical ionization mode.
开发了一种监测尿液中4,4'-亚甲基双（2-氯苯胺）（MOCA）的分析方法。尿样中的MOCA提取物用五氟丙酸酐衍生化，随后通过薄层色谱法净化，然后用配备电子捕获检测器的气相色谱仪进行分析。在定量过程中，使用七氟丁酸酐衍生化的MOCA作为内标。该方法表明，通过使用薄层色谱法进行样品净化，可有效减少分析干扰。尿液中添加水平为7.5、22和62.5微克/立方分米的MOCA回收率均超过90%，检测限确定为1微克/立方分米。通过使用负离子化学电离模式的气相色谱-质谱仪对尿样中的MOCA进行确证。
