高效液相色谱-串联质谱法测定成人外用中药制品中非法添加14种局部麻醉药

Determination of 14 illegal additive local anesthetics in Chinese herbal products for adult topical use by high performance liquid chromatography-tandem mass spectrometry

样品经甲醇溶剂超声提取,采用Thermo Accucore RP-MS柱(100 mm×2.7 mm,2.6μm)分离,以甲醇和乙酸铵溶液作为流动相进行梯度洗脱,预设多反应监测(sMRM)模式进行定性与定量分析。结果显示,14种局部麻醉药在各自线性范围内,相关系数(R2)均大于0.9980,检出限为0.2~1 mg/kg,定量限为0.5~2.5 mg/kg,3个加标水平的回收率为77.8%~122.1%,相对标准偏差为0.9%~8.2%。采用此方法对44批样品进行快速筛查,检出9批样品含有一种或多种非法添加药物,被检出药物为利多卡因和丁卡因。该方法适用于成人外用中药制品中非法添加局部麻醉药的定性及定量分析。

Samples were extracted by methanol with ultrasound extraction,and separated on a Thermo Accucore RP-MS column(100 mm×2.7 mm,2.6μm)through gradient elution with methanol and ammonium acetate solution as mobile phase.A scheduled multiple reaction monitoring in positive mode was adopted in mass spectrometry acquisition.As a result,the 14 local anesthetics showed good linearities with all correlation coefficients(R2)above 0.9980 in their linear ranges.The limits of detection(LODs)for the 14 local anesthetics were 0.2-1 mg/kg,and the limits of quantification(LOQs)were 0.5-2.5 mg/kg.Recoveries for the analytes at three spiked levels ranged from 77.8%to 122.1%,with the relative standard deviations(RSDs)in the range of 0.9%-8.2%.Liduokayin and tetracaine were detected in 9 batches(44 batches in total)samples.The developed method can be used for the qualitative and quantitative determination of the illegal additive local anesthetics in Chinese herbal products for adult ropical use.