A simple, rapid, sensitive and specific gas chromatography–tandem mass spectrometry (GC–MS/MS) method was developed for quantitation of salbutamol in human urine using salbutamol-d3 as the internal standard. The processing of urines samples includes deconjugation with enzymatic hydrolysis, solid phase extraction procedure utilizing XAD2 column and liquid–liquid extraction accompanied by the derivatization by means of MSTFA/IODO–TMS/DTE mixture. The GC column was a HP Ultra-1 (17 m × 0.22 mm × 0.11 μm) used to separate the peak of interest. The data for GC–MS/MS were acquired and processed utilizing GC Labs Solution and Insight GCMS Software. The detection of spectra was performed on TQ 8050. This method included a chromatographic run of 13.67 min and the linearity was found over the concentration range of 250–2000 ng/mL with a regression coefficient (r2) of 0.99. The coefficient of variation for intra and interday assay precision was between 1.85 and 2.85% and the accuracy was between 95.50 and 107.04% for low quality control (QC), medium QC and high QC. The recovery was adequate to reliable detect the analyte at or below the level recommended by the World Anti-Doping Agency i.e., threshold 1000 ng/mL. The limit of detection and limit of quantification were found to be 10 and 100 ng/mL, respectively. The expanded measurement uncertainty (Uexp%) was found to be 8.28%.

中文翻译：

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气相色谱-串联质谱法定量人尿液中沙丁胺醇的测量不确定度和验证

以沙丁胺醇-d3为内标，开发了一种简单、快速、灵敏且特异的气相色谱-串联质谱（GC-MS/MS）方法，用于定量人尿液中的沙丁胺醇。尿液样品的处理包括酶解解离、利用 XAD2 柱的固相萃取程序以及液-液萃取并伴随 MSTFA/IODO-TMS/DTE 混合物的衍生化。GC 柱是 HP Ultra-1 (17 m × 0.22 mm × 0.11 μm)，用于分离感兴趣的峰。GC-MS/MS 数据是利用 GC Labs Solution 和 Insight GCMS 软件获取和处理的。光谱检测在 TQ 8050 上进行。该方法包括 13.67 分钟的色谱运行，在 250–2000 ng/mL 的浓度范围内呈线性，回归系数 (r2) 为 0.99。低质量控制 (QC)、中 QC 和高 QC 的日内和日间测定精度的变异系数在 1.85% 至 2.85% 之间，准确度在 95.50% 至 107.04% 之间。回收率足以可靠地检测处于或低于世界反兴奋剂机构建议水平（即阈值 1000 ng/mL）的分析物。检测限和定量限分别为 10 ng/mL 和 100 ng/mL。扩展测量不确定度 (Uexp%) 为 8.28%。