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    超声提取-超高效液相色谱-串联质谱法测定毛发中常见毒品及代谢物的含量

    Determination of Common Drugs and Metaboliteies in Hair by UHPLC-MS/MS with Ultrasonic Extraction

    • 摘要: 建立了超声提取-超高效液相色谱-串联质谱法(UHPLC-MS/MS)测定毛发中常见毒品及代谢物含量的方法。称取洗涤(水、二氯甲烷、丙酮依次振荡洗涤各1次)并晾干后的毛发样品40~60 mg,将其剪成约1 mm小段,加入3.2 mm的破碎珠6颗,冷冻破碎5 min;再称取破碎后的毛发样品20 mg,加入1 mL甲醇,于0℃冰水浴中超声提取20 min,上清液用0.25 μm有机滤膜过滤,滤液供UHPLC-MS/MS测定。结果显示:O6-单乙酰吗啡(6-AM)、吗啡(MOR)、氯胺酮(K粉)、甲基苯丙胺(MAMP)、苯丙胺(AMP)、可卡因(COC)、苯甲酰爱康宁(BZE)、3,4-亚甲双氧甲基苯丙胺(MDMA)、3,4-亚甲双氧苯丙胺(MDA)、3,4-亚甲双氧乙基苯丙胺(MDEA)、可待因(COD)、去甲氯胺酮(NK)、Δ9-四氢大麻酚(THC)、大麻二酚(CBD)、大麻酚(CBN)等15种目标物的质量分数在一定范围内与其对应的峰面积呈线性关系,BZE、THC、CBD、COC、CBN的检出限(3S/N)均为0.001 ng·mg-1,6-AM、MOR、K粉、MAMP、AMP、MDMA、MDA、MDEA、COD、NK的检出限(3S/N)均为0.004 ng·mg-1;按照标准加入法对3个浓度水平的空白样品溶液进行测定,回收率为73.3%~97.8%,测定值的相对标准偏差(RSD,n=10)为4.3%~14%。方法用于实际样品的检测,测定结果与司法鉴定技术规范的测定结果一致。

       

      Abstract: A method for determination of common drugs and metabolites in hair by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) with ultrasonic extraction was established. Hair sample of 40-60 mg was dried after washing by water, dichlorocarbon and acetone. The hair sample was cut into 1 mm segments, and 6 broken beads of 3.2 mm were added. The sample was broken cryogenically for 5 min. Then methanol of 1 mL was added into broken hair sample of 20 mg, and ultrasonic extraction was carried out at 0℃ for 20 min in an ice-water bath. The supernatant was filtered by 0.25 μm organic filter membrane and determined by UHPLC-MS/MS. It was showed that linear relationships between mass fractions of O6-monoacetylmorphine (6-AM), morphine (MOR), ketamine, methamphetamine (MAMP), amphetamine (AMP), cocaine (COC), benzoyl-iconine (BZE), 3,4-methylene dioxymethamphetamine (MDMA), 3,4-methylene dioxyamphetamine (MDA), 3,4-methylene dioxyethyl amphetamine (MDEA), codeine (COD), normethylene ketamine (NK), tetrahydrocannabinol (THC), cannabidiol (CBD), cannabinol (CBN) and their peak areas were kept in definite ranges, with detection limits (3S/N) of 0.001 ng·mg-1 for BZE, THC, CBD, COC, CBN, and 0.004 ng·mg-1 for 6-AM, MOR, ketamine, MAMP, AMP, MDMA, MDA, MDEA, COD, NK. Recovery test was made on blank samples at 3 concentration levels by standard addition method, giving results in the range of 73.3%-97.8%, and RSDs (n=10) of the determined values were ranged from 4.3% to 14%. This method has been used to test substantial samples, and the results were consistent with those of standards of forensic science.

       

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