Laboratoire National de Santé, Toxicology Department, Avenue de la Faïencerie 162a, L-1511, Luxembourg.
Forensic Sci Int. 2012 Nov 30;223(1-3):119-24. doi: 10.1016/j.forsciint.2012.08.014. Epub 2012 Aug 30.
A sensitive and accurate LC-MS/MS method for the identification and quantification of 5 oral anti-diabetics (glipizide, glibenclamide, gliclazide, gliquidone and metformin) in serum and hair was developed using glibornuride as the internal standard. We have developed a rapid and robust extraction procedure by using acetonitrile for serum protein precipitation and methanol for the extraction of anti-diabetics from hair. Anti-diabetics (ADs) were separated by UPLC over a C18 column and detection was performed on a Waters Xevo TQ MS mass spectrometer in positive ionization mode using electrospray ionization. Each AD was identified by three specific ion transitions in multiple reaction monitoring (MRM) mode. The method was validated according to international guidelines. For all compounds the variation coefficient (CV) was <20%, and accuracies ranged from 85 to 115% in serum and hair. The limits of detection (LODs) were <1.5 ng/mL for all ADs in serum and <3.59 pg/mg in hair. Recoveries varied from 56.41% (gliclazide) to 67.58% (glipizide) in serum and from 68% (gliclazide) to 91.2% (metformin) in hair. The method was successfully applied to quantify ADs in serum of 33 patients and in hair of 15 patients.
建立了一种灵敏、准确的 LC-MS/MS 法，用于血清和头发中 5 种口服抗糖尿病药物（格列吡嗪、格列本脲、格列齐特、格列喹酮和二甲双胍）的鉴定和定量，以格列本脲为内标。我们开发了一种快速、稳健的提取方法，采用乙腈沉淀血清蛋白，甲醇提取头发中的抗糖尿病药物。采用 UPLC 在 C18 柱上分离抗糖尿病药物，在正离子模式下，用电喷雾电离在 Waters Xevo TQ MS 质谱仪上进行检测，采用多反应监测（MRM）模式进行检测。每种 AD 均通过三个特定的离子跃迁进行鉴定。该方法按照国际指南进行了验证。对于所有化合物，变异系数（CV）<20%，血清和头发中的准确度在 85%至 115%之间。所有 AD 在血清中的检测限（LOD）均<1.5 ng/mL，在头发中的检测限均<3.59 pg/mg。回收率在血清中从 56.41%（格列齐特）到 67.58%（格列吡嗪）不等，在头发中从 68%（格列齐特）到 91.2%（二甲双胍）不等。该方法成功应用于 33 例患者血清和 15 例患者头发中 ADs 的定量。
