摘要
目的建立HPLC—MS/MS分析方法测定人血浆中的金刚烷胺浓度,并用于研究健康受试者口服氨酚咖黄烷胺片后金刚烷胺的药动学。方法血浆经乙醚一二氯甲烷(4:1,V/y)提取,采用C18柱为分析柱,甲醇-10mmol·L^-1醋酸铵溶液一冰醋酸(60:40:0.08,V/V/V)为流动相,流速1.0mL·min^-1,柱后分流,0.2mL·min^-1进入质谱,柱温35℃。质谱检测方式:多反应离子监测,选择监测的离子为m/z 152→m/z 135(金刚烷胺)和m/z275→m/z 230(内标物,氯苯那敏)。结果金刚烷胺的线性范围为1—200μg·L^-1(r=0.9999),血浆中金刚烷胺的最低定量限达1μg·L^-1(RS,N〉10),回收率〉80%。结论本法简便、准确、灵敏度高,适用于金刚烷胺的药动学研究。
AIM To develop an LC-MS/MS assay to determine amantadine in human plasma and investigate the pharmacokinetics of amantadine after oral administration of the compound preparation. METHODS The plasma samples were extracted with ethyl ether-dichlormethane (4: 1, V/V). The separation was carried out on a Shimadzu ODS column (150 mm × 4.6 mm, 5μm) at 35 ℃. The mobile phase consisted of methanol, 10 mmol·L^-1 ammonium acetate and acetic acid (60:40:0.08, V/V/V), runrfing at a flow rate of 1.0 mL·min^-1. After separation, the mobile phase was splitted and 0.2 mL·min^-1 was into MS. LC-MS/MS was performed in the MRM mode using target ions at m/z 152→ m/z 135 for amantadine and m/z 275→m/z 230 for chlorphenamine. RESULTS The linear calibration curve was obtained in the concentration range of 1 -200μg· L^-1( r = 0.999 9). The lowest limit of quantification of amantadine in plasma was 1μg· L^-1. The average recovery was more than 80%. CONCLUSION The assay is proved to be sensitive, accurate and convenient. The method can be used for the pharmacokinetic research of amantadine.
出处
《中国临床药学杂志》
CAS
2008年第2期109-111,共3页
Chinese Journal of Clinical Pharmacy