柱前衍生-气质联用法同时测定人血浆中水杨酸、阿司匹林和氯吡格雷的浓度
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摘要
目的:建立一种同时测定人血浆中水杨酸、阿司匹林和氯吡格雷浓度的GC-MS方法。方法:使用SH-Rxi-5Sil (30m×0.25mmID,0.25μm)气相色谱柱,以甲醇作为样品溶剂同时也是甲酯衍生化试剂,在气相进样口高温衬管内衍生化并气相分离,质谱定量检测样本中的水杨酸和阿司匹林衍生物,以及氯吡格雷的含量。结果:水杨酸、阿司匹林和氯吡格雷分别在0.26～127.5μg·mL-1、1.93～965μg·mL-1和5.45～2180ng·mL-1范围内线性良好,三种待测物的定量下限分别可达0.26,1.93,5.45ng·mL-1。结论:该方法所用的血浆样本量少,操作相对简便污染小,测定周期短,对水杨酸、阿司匹林和氯吡格雷的测定结果稳定性和重复性良好,可以作为临床血药浓度检测的方法推广。
OBJECTIVE To establish a GC-MS method for simultaneous determination of salicylic acid, aspirin, and clopidogrel concentrations in human plasma. METHODS SH-Rxi-5Sil(30 m×0.25 mm ID, 0.25 μm) GC column was used with methanol as a sample solvent and also as a methyl ester derivatization reagent, derivatization was performed in the high-temperature liner of the gas phase injection port, followed by gas phase separation, then mass spectrometry was used to quantify the contents of salicylic acid, aspirin derivatives and, clopidogrel. RESULTS Salicylic acid, aspirin,and clopidogrel had good linearity in the ranges of 0.26 to 127.5 μg·mL-1, 1.93 to 965 μg·mL-1, and 5.45 to 2180 ng·mL-1,respectively, and the lower limits of quantification of the three analytes reached 0.26 μg·mL-1, 1.93 μg·mL-1, and 5.45ng·mL-1. CONCLUSION The method is relatively simple to operate and less pollutant, and has a short assay period. The stability and reproducibility of the determination results of salicylic acid, aspirin, and Cclopidogrel are good, and can be used as a method for the detection of clinical blood drug concentration.
OBJECTIVE To establish a GC-MS method for simultaneous determination of salicylic acid, aspirin, and clopidogrel concentrations in human plasma. METHODS SH-Rxi-5Sil(30 m×0.25 mm ID, 0.25 μm) GC column was used with methanol as a sample solvent and also as a methyl ester derivatization reagent, derivatization was performed in the high-temperature liner of the gas phase injection port, followed by gas phase separation, then mass spectrometry was used to quantify the contents of salicylic acid, aspirin derivatives and, clopidogrel. RESULTS Salicylic acid, aspirin,and clopidogrel had good linearity in the ranges of 0.26 to 127.5 μg·mL-1, 1.93 to 965 μg·mL-1, and 5.45 to 2180 ng·mL-1,respectively, and the lower limits of quantification of the three analytes reached 0.26 μg·mL-1, 1.93 μg·mL-1, and 5.45ng·mL-1. CONCLUSION The method is relatively simple to operate and less pollutant, and has a short assay period. The stability and reproducibility of the determination results of salicylic acid, aspirin, and Cclopidogrel are good, and can be used as a method for the detection of clinical blood drug concentration.
引文
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[9] ZHAO Kun, MEI Sheng-hui, LI Xin-gang, et al. An UPLC method for determination of aspirin and salicylic acid in human plasma[J]. Chin Hosp Pharm J(中国医院药学杂志),2017, 37(3):207-210+243.
[10] Peer CJ, Spencer SD, VanDenBerg DA, et al. A sensitive and rapid ultra HPLC-MS/MS method for the simultaneous detection of clopidogrel and its derivatized active thiol metabolite in human plasma[J]. J Chromatogr B Analyt Technol Biomed Life Sci, 2012, 880(1):132-139.
[11] ZHANG Kailong, SHEN Tingting, TAN Zhiwen, et al.Hydrolysis Kinetics of Acetylsalicylic Acid[J]. Research and Exploration in Laboratory(实验室研究与探索),2017,36(5):32-35.
[2] Eriksson P. Creative cost-effectiveness analysis of CAPRIEdata-dust in our eyes[J]. The American journal of medicine, 2005, 118(2):199-200.
[3] Tantray JA, Reddy KP, Jamil K, et al. Pharmacodynamic and cytogenetic evaluation in CYP2C19*2 and CYP2C19*3allelomorphism in south indian population with clopidogrel therapy[J]. Int J Cardiol, 2017, 229:113-118.
[4] Bykov K, Schneeweiss S, Donneyong MM, et al. Impact of an interaction between clopidogrel and selective serotonin reuptake inhibitors[J]. Am J Cardiol,2017,119(4):651-657
[5] Scott SA,Sangkuhl K, Stein CM, et al. Clinical pharmacogenetics implementation consortium guidelines for cyp2c19 genotype and clopidogrel therapy:2013 update[J].Clin Pharmacol Ther, 2013, 94:317-323.
[6] Wysham C H, Kirkman M S. Response to Comment on:American Diabetes Association. Standards of Medical Care in Diabetes-2011. Diabetes Care 2011; 34(Suppl. 1):S11-S61[J]. Diabetes Care,2011,34(5):e54-e54.
[7] Ma W, Liang Y, Zhu J, et al. Meta-analysis appraising high maintenance dose clopidogrel in patients who underwent percutaneous coronary intervention with and without highon-clopidogrel platelet reactivity[J]. Am J Cardiol, 2015,115(5):592-601.
[8] CHEN Minchun, LU Chengtao, JIA Yanyan, et al.Determination of clopidogrel in human plasma by LC-MS/MS and its application to bioequiavailability[J]. Chin Hosp Pharm J(中国医院药学杂志),2012, 32(6):421-424.
[9] ZHAO Kun, MEI Sheng-hui, LI Xin-gang, et al. An UPLC method for determination of aspirin and salicylic acid in human plasma[J]. Chin Hosp Pharm J(中国医院药学杂志),2017, 37(3):207-210+243.
[10] Peer CJ, Spencer SD, VanDenBerg DA, et al. A sensitive and rapid ultra HPLC-MS/MS method for the simultaneous detection of clopidogrel and its derivatized active thiol metabolite in human plasma[J]. J Chromatogr B Analyt Technol Biomed Life Sci, 2012, 880(1):132-139.
[11] ZHANG Kailong, SHEN Tingting, TAN Zhiwen, et al.Hydrolysis Kinetics of Acetylsalicylic Acid[J]. Research and Exploration in Laboratory(实验室研究与探索),2017,36(5):32-35.