固相萃取-液相色谱-串联质谱法检测血液中海洛因及其代谢产物

张松; 曹峻华; 刘文文

doi:10.7538/zpxb.youxian.2015.0020

固相萃取-液相色谱-串联质谱法检测血液中海洛因及其代谢产物

1.
重庆市公安局交通管理局,重庆400054
2.
重庆市公安局物证鉴定中心,重庆400021

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- 刊出日期: 2015-07-19

Determination of Heroin and Its Metabolites in Addicts’ Blood by Solid Phase Extraction and LC-MS/MS

1.
Chongqing -Traffic Management Bureau, Chongqing 400054, China
2.
Chongqing Institute of Forensic Science, Chongqing 400021, China

摘要

摘要: 建立了固相萃取-液相色谱-串联质谱（SPE-LC-MS/MS）法分析吸毒者血样中的O⁶-单乙酰吗啡、吗啡、3-β-D-葡萄糖醛酸吗啡。以3-β-D-葡萄糖醛酸吗啡-d₃为内标，选取Oasis HLB为固相萃取柱，Atlantis^TMdC18（150 mm×3.9 mm×5 μm）色谱柱为分析柱，采用甲醇-0.1%甲酸水溶液为流动相进行梯度洗脱；采用电喷雾正离子电离源，多反应监测（MRM）扫描方式，通过两对母离子/子离子和保留时间定性定量检测目标化合物。结果表明：血样中O⁶-单乙酰吗啡、吗啡、3-β-D-葡萄糖醛酸吗啡的检测限为3~5 μg/L，线性关系良好，相关系数均在0.997 5以上；添加50、500、1 000 μg/L加标水平后，O⁶-单乙酰吗啡、吗啡、3-β-D-葡萄糖醛酸吗啡的平均回收率为80.6%~98.9%，准确度为-7.3%~9.1%。该方法具有较高的灵敏度和选择性，可用于实际案件中海洛因及其代谢产物的检测。
- 液相色谱-串联质谱法（LC-MS/MS） /
- 固相萃取（SPE） /
- O⁶-单乙酰吗啡 /
- 吗啡 /
- 3-β-D-葡萄糖醛酸吗啡
Abstract: O⁶-Monoacetylmorphine, morphine, morphine-3-β-D-glucuronide in addicts’ blood samples were analyzed by solid phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted by extraction column (Oasis HLB), and then were flushed into the analytical column (Atlantis^TM dC18 (150 mm×3.9 mm×5 μm)) with methanol and water containing formic acid as mobile phase and morphine-3-β-D-glucuronide-d₃as internal standard. The positive electric spray ionization, multiple reaction monitoring (MRM) mode were applied to analyze target compounds. Identification was based on the compound’s retention time and two pairs of precursor-to-product ion transitions. The results show that the limit of detections are 3-5 μg/L for morphine, O⁶-monoacetylmorphine and morphine-3-β-D-glucuronide. The linear relationship is well, and the linear correlation coefficient is greater than 0.997 5. The average recoveries are 80.6%-98.9% with the spiked levels of 50, 500, 1 000 μg/L, and the accuracies are -7.3%-9.1%. The method has high sensitivity and selectivity, which is suitable for analyzing the heroin and its metabolites in addicts’ blood samples.
- liquid chromatography-tandem mass spectrometry (LC-MS/MS) /
- solid phase extraction (SPE) /
- O⁶-monoacetylmorphine /
- morphine /
- morphine-3-β-D-glucuronide

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参考文献(12)

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固相萃取-液相色谱-串联质谱法检测血液中海洛因及其代谢产物

计量

出版历程

Determination of Heroin and Its Metabolites in Addicts’ Blood by Solid Phase Extraction and LC-MS/MS

计量

出版历程

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