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    毛细管固相微萃取-超高效液相色谱-串联质谱法测定血浆中麻醉精神药物

    Determination of Abused Drugs in Human Plasma by In-Tube SPME-UHPLC-MS/MS

    • 摘要: 提出了毛细管固相微萃取-超高效液相色谱-串联质谱法测定血浆中麻醉精神药物含量的方法.取样品1 mL,加硼砂缓冲液2 mL混匀,离心,上清液转入注射器针管中,接内壁固定有DB-5毛细管色谱柱的不锈钢针头,置于注射泵上以200 μL·min-1流量排出样品,用1 mL水冲洗针头,再用50 μL乙腈洗脱2 min.以梯度洗脱-电喷雾正离子源-多反应监测测定洗脱液中药物成分.16种药物的检出限小于10 μg·L-1,18种药物的检出限在10~50 μg·L-1之间,3种药物的检出限不小于77 μg·L-1,5种药物未能检出.血浆中37种药物回收率在4.0%~93.5%之间,相对标准偏差(n=6)在0.80%~13%之间.76起案例样品中检出31例.

       

      Abstract: A method of in-tube SPME-UPLC-MS/MS was used to measure abused drugs in plasma. 1 mL of plasma was mixed well with 2 mL of sodium borate buffer,and then centrifuged. The supernatant was taken into a sampler connected with a stainless steel needle fixed with DB-5 capillary column and then injected at a speed of 200 μL·min-1 by a syringe pump. The needle was washed using 1 mL of water and then eluted for 2 min using 50 μL of acetonitrile as eluent. Gradient elution,ESI+ and MRM were adopted in UPLC-MS/MS detection. The detection limits were below 10 μg·L-1 for 16 drugs,and 10-50 μg·L-1 for 18 drugs,and ≥77 μg·L-1 for 3 drugs. 5 drugs were not detected. The recovery rates and RSD′s (n=6) for 37 drugs in plasma were in the range of 4.0%-93.5% and 0.80%-13%,respectively. Drugs were detected in 31 out of the 76 plasma samples by this method.

       

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