Jaroszewski J W, Berenstein D, Sløk F A, Simonsen P E, Agger M K
Department of Medicinal Chemistry, Royal Danish School of Pharmacy, Copenhagen, Denmark.
J Pharm Biomed Anal. 1996 Mar;14(5):543-9. doi: 10.1016/0731-7085(95)01664-3.
1H-NMR spectroscopy is a convenient method for determination of diethylcarbamazine (DEC) in urine, and can be used to monitor medication with the drug. Urine samples were mixed with 10% of deuterium oxide as a spectrometer field frequency lock, which is the only sample pretreatment required. Tailored excitation with the 1331 pulse was used for water peak suppression. The quantification of DEC was carried out with the triplet of the N-ethyl group, for which the T1 relaxation time was 1 s. In aqueous solutions, amounts below 1 microgram ml-1 of DEC could be easily detected. In urine, the detectability depended on the level of chemical noise but was better than 10 micrograms ml-1. The accuracy and precision of the method were better than 15%. Analysis of urine from volunteers receiving a single therapeutic dose of DEC (6 mg kg-1 body weight orally) showed that the drug was eliminated in unchanged form during 2 days, in agreement with earlier results. The concentration of DEC in urine several hours after the intake exceeded 100 micrograms ml-1 making the 1H-NMR assay rapid and easy. No significant amounts of the N-oxide of DEC could be detected.
1H-核磁共振光谱法是测定尿液中二乙碳酰嗪（DEC）的一种便捷方法，可用于监测该药物的用药情况。尿液样本与10%的氧化氘混合作为光谱仪场频锁，这是唯一需要的样本预处理。使用1331脉冲进行定制激发以抑制水峰。DEC的定量分析采用N-乙基的三重峰进行，其T1弛豫时间为1秒。在水溶液中，DEC含量低于1微克/毫升时很容易被检测到。在尿液中，可检测性取决于化学噪声水平，但优于10微克/毫升。该方法的准确度和精密度优于15%。对接受单次治疗剂量DEC（口服6毫克/千克体重）的志愿者尿液进行分析表明，该药物在2天内以原形排出，与早期结果一致。摄入后数小时尿液中DEC的浓度超过100微克/毫升，使得1H-核磁共振测定法快速且简便。未检测到大量的DEC N-氧化物。
