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目的:建立高效液相色谱-三重四级杆质谱联用(LC-MS/MS)法检测人头发中利培酮(RIP)及其代谢物9-羟利培酮(9-OH-RIP)含量的方法。方法:采用同位素内标氘4-利培酮(RIP-d4)及氘4-9-羟利培酮(9-OH-RIP-d4),流动相A为10 mmol/L醋酸胺溶液(甲酸调p H值为4.0),流动相B为乙腈,A/B=70/30,流速为0.3 m L/min,等度洗脱4.00 min。色谱柱为安捷伦Zorbax SB C18(2.1×50 mm,1.8μm),柱温30℃。准确称取20 mg丙酮清洗过晾干剪碎成粉末的头发样本,加1N氢氧化钠(Na OH)超声2 h,等量酸中和后,加200μL1N氢氧化钠溶液及5.0 m L的甲基叔丁基醚(MTBE)提取涡旋1分钟,3000×g离心5 min后取上清液在40度水浴下氮气吹干后用100μL流动相复溶,进样2μL经LC-MS/MS检测。MRM监测离子对:RIP:m/z 411.2→191.0,9-OH-RIP:m/z 427.2→207.1,RIP-d4:m/z 415.2→195.2,9-OH-RIP-d4:m/z 431.2→211.1。结果:利培酮及9-羟利培酮线性范围分别为0.5-25 ng/mg,0.0025-0.15 ng/mg,提取回收率均>70.0%,方法回收率均在85.0%-115.0%之间,线性r均>0.999,精密度和重现性RSD均<15%。结论:本研究建立了采用LC-MS/MS法检测人头发中利培酮及9-羟利培酮含量的方法,该法快速、简单、准确、重现性好。
OBJECTIVE: To establish a method for the determination of risperidone (RIP) and its metabolite 9-OH-RIP in human hair by high performance liquid chromatography-triple quadrupole mass spectrometry (LC-MS / MS) Method of content. Methods: The isotope internal standard deuterium 4-risperidone (RIP-d4) and deuterium 4-9-hydroxy-risperidone (9-OH-RIP-d4) were used.The mobile phase A was 10 mmol / L ammonium acetate solution PH = 4.0), mobile phase B was acetonitrile, A / B = 70/30 with a flow rate of 0.3 mL / min and an isocratic elution of 4.00 min. The column was Agilent Zorbax SB C18 (2.1 × 50 mm, 1.8 μm) with a column temperature of 30 ° C. Accurately weighed 20 mg of acetone washed dried hair cut into powder hair samples, plus 1N sodium hydroxide (NaOH) ultrasound 2 h, the same amount of acid neutralization, add 200μL 1N sodium hydroxide solution and 5.0 m L of a (MTBE) for 1 minute. After centrifugation at 3000 × g for 5 min, the supernatant was dried under nitrogen in a 40 ° water bath and then reconstituted with 100 μL of mobile phase. 2 μL of the solution was analyzed by LC-MS / MS Detection. MRM monitoring ion pair: RIP: m / z 411.2 → 191.0,9-OH-RIP: m / z 427.2 → 207.1, RIP-d4: m / z 415.2 → 195.2, 9-OH-RIP-d4: m / z 431.2 → 211.1. Results: The linear ranges of risperidone and 9-hydroxyrisperidone were 0.5-25 ng / mg and 0.0025-0.15 ng / mg, respectively, and the recovery rates were both> 70.0%. The recovery rates were between 85.0% and 115.0% , Linear r> 0.999, precision and reproducibility RSD <15%. Conclusion: This study established a method for the determination of risperidone and 9-hydroxyrisperidone in human hair by LC-MS / MS. The method is rapid, simple, accurate and reproducible.