Citation: LYU Yufan, WANG Jifen, CHANG Jing, LI Chao, PENG Shanshan. Determination of morphine and 6-monoacetylmorphine in putrefied blood using ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2019, 37(1): 80-86. doi: 10.3724/SP.J.1123.2018.08004 shu

Determination of morphine and 6-monoacetylmorphine in putrefied blood using ultra performance liquid chromatography-tandem mass spectrometry

1.
School of Criminal Science and Technology, People's Public Security University of China, Beijing 100038, China;
2.
Institute of Forensic Science, Ministry of Public Security, Beijing 100038, China

Received Date: 2 August 2018

Fund Project: National Key Research and Development Program (No.2017YFC0803604-2).

This study was performed to develop an ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method to detect and quantify morphine and 6-monoacetylmorphine in putrefied blood for forensic toxicological purposes. A modified QuEChERS method was implemented as follows:extraction of morphine and 6-monoacetylmorphine from putrefied blood was performed with an acetonitrile-water (4:1, v/v) mixture, and 30 mg NaCl and 60 mg anhydrous MgSO₄ were subsequently added as salting out agents to induce phase separation. The supernatant was cleaned by adding 25 mg primary secondary amine sorbent (PSA) and 25 mg anhydrous MgSO₄. Separation of the target compounds was performed using a ZORBAX Eclipse Plus C₁₈ column by UPLC over a 4 min gradient elution where 0.01% (v/v) ammonium hydroxide buffer (A) and acetonitrile (B) were used as the mobile phase. MS/MS was used in positive electrospray ionization (ESI⁺) mode and multiple-reaction monitoring (MRM) was performed to detect the target drugs. This method achieved satisfactory recoveries (R) for morphine and 6-monoacetylmorphine with mean recovery values ranging from 81.84% to 103.44% and 81.03% to 104.46% respectively. The developed method also provided efficient purification of the sample from endogenous interferences with matrix effect (ME) ranging from 83.04% to 107.61%. The method was validated and the limit of detection (LOD) and limit of quantification (LOQ) were 1 and 5 μg/L, respectively, for both compounds and the precision with RSD ranged from 1% to 12%. This method proved to be quick, sensitive, rugged, and suitable for the analysis of illegal drugs in putrefied whole blood.
- QuEChERS,
- ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),
- morphine,
- 6-monoacetylmorphine,
- putrefied blood
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1.
沈阳化工大学材料科学与工程学院沈阳 110142