| 孙秀佳 林治光 任娟娟 蒋平 刘红梅 李春波 李华芳.LC-MS/MS法检测人头发中利培酮及其代谢物9-羟利培酮含量的实验研究[J].,2015,15(12):2221-2224 |
| LC-MS/MS法检测人头发中利培酮及其代谢物9-羟利培酮含量的实验研究 |
| Determination of Risperidone and Its Metabolite of 9-hydroxyrisperidone inHair by LC-MS/MS |
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| DOI： |
| 中文关键词: 利培酮 9-羟利培酮 LC-MS/MS 药物浓度 头发 |
| 英文关键词: Risperidone 9-hydroxy-risperidone LC-MS/MS Drug concentration Hair |
| 基金项目:国家" 重大新药创制" 科技重大专项（2012ZX09303-003）；上海市卫生系统优秀人才（XBR2011049）；
上海市卫生系统优秀学科带头人培养计划（XBR2011005），上海市精神卫生中心院级课题（2012-YJ-09） |
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| 中文摘要: |
| 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pH值为4.0)，流动相B 为乙腈，A/B=70/30，流速为0.3 mL/min，等度洗脱4.00 min。色谱柱为安捷伦Zorbax SB
C18(2.1× 50 mm，1.8 um)，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(NaOH)超声2 h，
等量酸中和后，加200 uL1N 氢氧化钠溶液及5.0 mL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100 uL 流动相复溶，进样2 滋L 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。 |
| 英文摘要: |
| Objective:To establish an HPLC-MS/MS method for the determination of risperidone (RIP) and its metabolite
9-hydroxy-risperidone (9-OH-RIP) in the hair.Methods:The isptope-labeled internal standards (risperidone-d4 and
9-hydroxyrisperidone-d4) were used. The mobile phase A 10 mm ammonium buffer (tune pH to 4.0 by formic acid); B: Acetonitrile;
A/B=70/30, flow rate of 0.3 mL/min, the analytical column was Agilent Zorbax SB C18 (2.1× 50 mm, 1.8 um), temperature was 30℃.
20 mg sample of hair was weighed accurately, which was washed by acetone and cuted into powder, ultrasonic for 2 h with added 1 mL
of 1N NaOH, then neutralized by 1 mL 1N HCL, added 200 uL 1N NaOH and 5.0 mLof Methyl Tertiary Butyl Ether vortex for 1 min,
3000 g centrifugation for 5 min, supernate was dried under 40℃ with nitrogen, and redissolved by 100 uL mobilephase，inject 2 uL into
LC-MS/MS. MRM: 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/z431.2→211.1.Results:The results showed that the linear was 0.5-25 ng/mg for RIP and 0.0025-0.15 ng/mg for 9-OH RIP, both of the linearly
dependent coefficient (r) were no less than 0.999, the recoverys of extraction >70.0 %, the recoverys of method was between 85.0 %and
115.0 %, and the RSDs of precision and accuracy were all no more than 15 %.Conclusion:A determination method of the concentration
of RIP and 9-OH-RIP in hair was established, which was simple and rapid, and had superior sensitivity and selectivity. |
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