Makhdoom Humera Shafi, Abid Ali Imran, Mujahid Majida, Afzal Saira, Sultana Kishwar, Hussain Nisar, Barkat Kashif
Faculty of Pharmacy, University of Lahore, Lahore, Pakistan.
Clinical and Forensic Toxicology Department, Chughtai Healthcare, Lahore, Pakistan.
Forensic Sci Med Pathol. 2024 Dec;20(4):1291-1302. doi: 10.1007/s12024-024-00795-7. Epub 2024 Mar 26.
Pheniramine is an over-the-counter antihistamine drug. Its accessibility and low cost made it more popular among drug abusers in Pakistan. In this study, pheniramine was quantified in both conventional and alternative specimens of twenty chronic drug abusers, aged 16-50 years, who were positive for pheniramine in comprehensive toxicological screening for drugs by gas chromatography with mass spectral detection in positive electron impact mode. Pheniramine was extracted from biological specimens using solid phase extraction and liquid chromatography tandem mass spectrometry was employed for quantification. Chromatographic separation was carried out on a Poroshell120EC-18 (2.1 mm × 50 mm × 2.7 µm) column using water-acetonitrile in formic acid (0.1%) mobile phase in gradient elution mode with 500 μL/min flow rate. Positive electrospray ionization mode and multi-reaction monitoring with ion transitions m/z 241.3 → 195.8 and 167.1 for pheniramine and m/z m/z 247.6 → 173.1 for pheniramine-d6 were employed. The quantification method showed good linear ranges of 2-1000 ng/mL in blood, urine, and oral fluid; 2-1000 ng/mg in hair and 5-1000 ng/mg in nail with ≥ 0.985% coefficient of linearity. The retention time of pheniramine was 3.0 ± 0.1 min. The detection and lower quantification limits were 1 ng/mL and 2 ng/mL for blood, urine, oral fluid and hair whereas 2.5 ng/mg and 5 ng/mg for nail, respectively. Mean extraction recovery and ionization suppression ranged 86.3-95.1% and -4.6 to -14.4% in the studied matrices. Intra-day and inter-day precision were 4.1-9.3% and 2.8-11.2%, respectively. Pheniramine levels in specimens of drug abusers were 23-480 ng/mL in blood, 72-735 ng/mL in urine, 25-379 ng/mL in oral fluid, 10-170 ng/mg in hair and 8-86 ng/mg in nail specimens. Alternative specimens are of utmost significance in clinical and medico-legal cases. In this study, authors compared matrix-matched calibration curves to blood calibration curve and obtained results within ± 10%; thereby justifying the use of blood calibration curve for urine, oral fluid, hair, and nail specimens.
非尼拉敏是一种非处方抗组胺药。其易获取性和低成本使其在巴基斯坦的药物滥用者中更受欢迎。在本研究中，对20名年龄在16至50岁的慢性药物滥用者的常规和替代样本中的非尼拉敏进行了定量分析，这些滥用者在采用正电子轰击模式的气相色谱 - 质谱检测进行的药物综合毒理学筛查中，非尼拉敏呈阳性。使用固相萃取从生物样本中提取非尼拉敏，并采用液相色谱 - 串联质谱法进行定量。色谱分离在Poroshell120EC - 18（2.1 mm×50 mm×2.7 µm）色谱柱上进行，流动相为含0.1%甲酸的水 - 乙腈，采用梯度洗脱模式，流速为500 μL/min。采用正电喷雾电离模式和多反应监测，非尼拉敏的离子跃迁为m/z 241.3→195.8和167.1，非尼拉敏 - d6的离子跃迁为m/z 247.6→173.1。该定量方法在血液、尿液和口腔液中的线性范围为2 - 1000 ng/mL；在毛发中为2 - 1000 ng/mg，在指甲中为5 - 1000 ng/mg，线性系数≥0.985%。非尼拉敏的保留时间为3.0±0.1分钟。血液、尿液、口腔液和毛发的检测限和最低定量限分别为1 ng/mL和2 ng/mL，而指甲的检测限和最低定量限分别为2.5 ng/mg和5 ng/mg。在所研究的基质中，平均提取回收率和电离抑制范围分别为86.3 - 95.1%和 - 4.6至 - 14.4%。日内和日间精密度分别为4.1 - 9.3%和2.8 - 11.2%。药物滥用者样本中的非尼拉敏水平在血液中为23 - 480 ng/mL，尿液中为72 - 735 ng/mL，口腔液中为25 - 379 ng/mL，毛发中为10 - 170 ng/mg，指甲样本中为8 - 86 ng/mg。替代样本在临床和法医学案例中具有极其重要的意义。在本研究中，作者将基质匹配校准曲线与血液校准曲线进行了比较，结果在±10%以内；从而证明了血液校准曲线可用于尿液、口腔液、毛发和指甲样本。
