中国药物应用与监测
中國藥物應用與鑑測
중국약물응용여감측
CHINESE JOURNAL OF DRUG APPLICATION AND MONITORING
2014年
5期
276-278
,共3页
赵冠人%申健%彭明丽%蒋南
趙冠人%申健%彭明麗%蔣南
조관인%신건%팽명려%장남
高效液相色谱-质谱联用%他克莫司%血药浓度
高效液相色譜-質譜聯用%他剋莫司%血藥濃度
고효액상색보-질보련용%타극막사%혈약농도
HPLC-MS/MS%Tacrolimus%Blood drug concentration
目的:建立测定人全血中他克莫司浓度的高效液相-质谱联用方法。方法:采用地西泮为内标,色谱柱为Agilent Poroshell 120 SB-C18柱(4.6 mm ×50 mm,2.7μm),流动相为乙腈-0.01 mol·L-1醋酸铵与0.5%甲酸的混合溶液,梯度洗脱,柱温40℃,流速0.7 mL·min-1,进样量5μL;采用多重反应监测(MRM)进行定量,ESI正离子方式进行检测,用于定量分析的监测离子为m/z 821.6→768.5(他克莫司)和m/z 285.1→193.1(内标地西泮)。结果:他克莫司在1.49~29.78 ng·mL-1的浓度范围内线性关系良好,准确度为95.19%~99.02%,批内与批间(3 d)RSD均小于10.00%。结论:该方法简便、快速、灵敏,适用于他克莫司治疗药物监测工作。
目的:建立測定人全血中他剋莫司濃度的高效液相-質譜聯用方法。方法:採用地西泮為內標,色譜柱為Agilent Poroshell 120 SB-C18柱(4.6 mm ×50 mm,2.7μm),流動相為乙腈-0.01 mol·L-1醋痠銨與0.5%甲痠的混閤溶液,梯度洗脫,柱溫40℃,流速0.7 mL·min-1,進樣量5μL;採用多重反應鑑測(MRM)進行定量,ESI正離子方式進行檢測,用于定量分析的鑑測離子為m/z 821.6→768.5(他剋莫司)和m/z 285.1→193.1(內標地西泮)。結果:他剋莫司在1.49~29.78 ng·mL-1的濃度範圍內線性關繫良好,準確度為95.19%~99.02%,批內與批間(3 d)RSD均小于10.00%。結論:該方法簡便、快速、靈敏,適用于他剋莫司治療藥物鑑測工作。
목적:건립측정인전혈중타극막사농도적고효액상-질보련용방법。방법:채용지서반위내표,색보주위Agilent Poroshell 120 SB-C18주(4.6 mm ×50 mm,2.7μm),류동상위을정-0.01 mol·L-1작산안여0.5%갑산적혼합용액,제도세탈,주온40℃,류속0.7 mL·min-1,진양량5μL;채용다중반응감측(MRM)진행정량,ESI정리자방식진행검측,용우정량분석적감측리자위m/z 821.6→768.5(타극막사)화m/z 285.1→193.1(내표지서반)。결과:타극막사재1.49~29.78 ng·mL-1적농도범위내선성관계량호,준학도위95.19%~99.02%,비내여비간(3 d)RSD균소우10.00%。결론:해방법간편、쾌속、령민,괄용우타극막사치료약물감측공작。
Objective:To establish the HPLC-MS/MS method for the determination of tacrolimus in human whole blood. Methods: The diazepam was used as internal standard. Tacrolimus was separated on an Agilent Poroshell 120 SB-C18 column (4.6 mm × 50 mm, 2.7μm) maintained at 40℃with acetonitrile-0.01 mol·L-1 ammonium acetate and 0.5%formic acid as mobile phase by gradient elution. The lfow rate was 0.7 mL·min-1, and the sample size was 5μL. Detection was performed with multiple reaction monitoring (MRM) scan mode measured with positive electrospray ionization (ESI+). The monitoring ions of tacrolimus and diazepam were m/z 821.6→768.5 and m/z 285.1→193.1, respectively. Results:Tacrolimus showed a good linear relationship in the range of 1.49-29.78 ng·mL-1. The accuracies were in the range of 95.19%-99.02%, both the inter-run and intra-run RSD (3 d) were less than 10.00%. Conclusion:The method is simple, rapid and sensitive, which can be used for the therapeutic drug monitoring of tacrolimus.