Kudo Keiko, Ikeda Noriaki, Kiyoshima Akiko, Hino Yukiko, Nishida Naoki, Inoue Naohide
Department of Forensic Pathology andSciences, Graduate School of Medical Sciences, Kyushu University, Fukuoka, Japan.
J Anal Toxicol. 2002 Mar;26(2):119-22. doi: 10.1093/jat/26.2.119.
A simple and reliable high-performance liquid chromatographic (HPLC) method for analyzing chlorhexidine in human serum was developed. After the addition of an internal standard, levomepromazine, 0.2 mL serum was deproteinized with 10% perchloric acid. The acidic supernatant was neutralized with 1M potassium carbonate solution, and the insoluble salt was removed by centrifugation. An aliquot of the supernatant was applied to HPLC with UV detection (260 nm). HPLC separation was achieved on a polymer-coated ODS column equilibrated with acetonitrile/water containing 0.05% trifluoroacetic acid, 0.05% heptafluorobutyric acid, and 0.1% triethylamine (40:60, v/v). The calibration curve was linear in the concentration range from 0.05 to 50.0 microg/mL, and the lower limit of detection was 0.05 microg/mL. The accuracy and precision of the method were evaluated at concentrations of 0.5 microg/mL and 5.0 microg/mL. The coefficients of variation ranged from 4.0 to 4.5%. The concentration of chlorhexidine in the serum of a patient who died after a suspected intravenous injection of chlorhexidine gluconate was determined.
建立了一种简单可靠的高效液相色谱（HPLC）法用于分析人血清中的洗必泰。加入内标物甲氧异丁嗪后，用10%高氯酸对0.2 mL血清进行脱蛋白处理。酸性上清液用1M碳酸钾溶液中和，通过离心除去不溶性盐。取上清液的一份等分试样进行带紫外检测（260 nm）的HPLC分析。在以含0.05%三氟乙酸、0.05%七氟丁酸和0.1%三乙胺的乙腈/水（40:60，v/v）平衡的聚合物涂层ODS柱上实现HPLC分离。校准曲线在0.05至50.0 μg/mL的浓度范围内呈线性，检测下限为0.05 μg/mL。在0.5 μg/mL和5.0 μg/mL的浓度下评估了该方法的准确性和精密度。变异系数范围为4.0%至4.5%。测定了一名疑似静脉注射葡萄糖酸氯己定后死亡患者血清中氯己定的浓度。
