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

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40~60mg,将其剪成约1mm小段,加入3.2mm的破碎珠6颗,冷冻破碎5min;再称取破碎后的毛发样品20mg,加入1mL甲醇,于0℃冰水浴中超声提取20min,上清液用0.25μm有机滤膜过滤,滤液供UHPLC-MS/MS测定。结果显示:O^(6)-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)、Δ^(9)-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0.001ng·mg^(-1),6-AM、MOR、K粉、MAMP、AMP、MDMA、MDA、MDEA、COD、NK的检出限(3S/N)均为0.004ng·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。

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 40-60mg was dried after washing by water,dichlorocarbon and acetone.The hair sample was cut into 1mm segments,and 6broken beads of 3.2mm were added.The sample was broken cryogenically for 5min.Then methanol of 1mL was added into broken hair sample of 20mg,and ultrasonic extraction was carried out at 0℃for 20 min in an ice-water bath.The supernatant was filtered by 0.25μm organic filter membrane and determined by UHPLC-MS/MS.It was showed that linear relationships between mass fractions of O^(6)-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 0.001ng·mg^(-1)for BZE,THC,CBD,COC,CBN,and 0.004ng·mg^(-1)for 6-AM,MOR,ketamine,MAMP,AMP,MDMA,MDA,MDEA,COD,NK.Recovery test was made on blank samples at 3concentration 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.