Lee Mei Jin, Ramanathan Surash, Mansor Sharif Mahsufi, Yeong Keng Yoon, Tan Soo Choon
Institute for Research in Molecular Medicine (INFORMM), Main Campus, Universiti Sains Malaysia, 11800, Penang, Malaysia.
Centre for Drug Research (CDR), Main Campus, Universiti Sains Malaysia, 11800, Penang, Malaysia.
Anal Biochem. 2018 Feb 15;543:146-161. doi: 10.1016/j.ab.2017.12.021. Epub 2017 Dec 14.
A method using solid phase extraction and liquid chromatography-tandem mass spectrometry to quantitatively detect mitragynine, 16-carboxy mitragynine, and 9-O-demethyl mitragynine in human urine samples was developed and validated. The relevant metabolites were identified using multiple reaction monitoring in positive ionization mode using nalorphine as an internal standard. The method was validated for accuracy, precision, recovery, linearity, and lower limit of quantitation. The intra- and inter-day accuracy and precision were found in the range of 83.6-117.5% with coefficient of variation less than 13%. The percentage of recovery for mitragynine, 16-carboxy mitragynine, and 9-O-demethyl mitragynine was within the range of 80.1-118.9%. The lower limit of quantification was 1 ng/mL for mitragynine, 2 ng/mL for 16-carboxy mitragynine, and 50 ng/mL for 9-O-demethyl mitragynine. The developed method was reproducible, high precision and accuracy with good linearity and recovery for mitragynine, 16-carboxy mitragynine, and 9-O-demethyl mitragynine in human urine.
建立并验证了一种使用固相萃取和液相色谱 - 串联质谱法定量检测人尿液样本中帽柱木碱、16 - 羧基帽柱木碱和9 - O - 去甲基帽柱木碱的方法。以烯丙吗啡为内标，在正离子模式下使用多反应监测对相关代谢物进行鉴定。该方法在准确性、精密度、回收率、线性和定量下限方面进行了验证。日内和日间的准确度和精密度在83.6 - 117.5%范围内，变异系数小于13%。帽柱木碱、16 - 羧基帽柱木碱和9 - O - 去甲基帽柱木碱的回收率在80.1 - 118.9%范围内。帽柱木碱的定量下限为1 ng/mL，16 - 羧基帽柱木碱为2 ng/mL，9 - O - 去甲基帽柱木碱为50 ng/mL。所建立的方法具有可重复性，对人尿液中的帽柱木碱、16 - 羧基帽柱木碱和9 - O - 去甲基帽柱木碱具有高精度和准确性，线性和回收率良好。
