今日药学

2021, v.31(05) 374-377

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HPLC-MS/MS法测定人血清和脑脊液中青霉素G的浓度
Determination of Penicillin Concentration in Human Serum and Cerebrospinal Fluid by HPLC-MS/MS

董琳;卢浩扬;邱萍英;温预关;
DONG Lin;LU Haoyang;QIU Pingying;WEN Yuguan;Pharmaceutical Department,The Affiliated Brain Hospital of Guangzhou Medical University,Guangzhou Huiai Hospital,Guangdong Engineering Technology Research Center for Translational Medicine of Mental Disorders;Hunan Agricultural University;Clinical Laboratory,The Affiliated Brain Hospital of Guangzhou Medical University,Guangzhou Huiai Hospital,Guangdong Engineering Technology Research Center for Translational Medicine of Mental Disorders;

摘要(Abstract):

目的采用高效液相色谱-串联质谱(HPLC-MS/MS)法建立测定人脑脊液和血清中青霉素G浓度方法。此方法可用于神经梅毒患者的脑脊液与血清中青霉素G浓度监测。方法以青霉素G-d7为内标,Agilent ZORBAX Eclipse XDB-C_(18)(4.6 mm×50 mm, 1.8μm)为分析柱,流动相为甲醇-水(82.5∶17.5,含3.5 mmol·L~(-1)甲酸铵),流速为0.5 mL·min~(-1),采用多重反应监测模式检测(MRM),通过三重四级杆串联质谱仪正离子模式分析青霉素G在血清和脑脊液浓度。结果青霉素G在血清中50~5 000 ng·mL~(-1)的浓度范围内线性关系良好(r=0.999 1,n=7),高、中、低浓度质控日内及日间精密度不高于11.26%,准确度在98.65%~103.46%内,提取回收率为99.64%,101.21%,105.22%;在脑脊液中10~1 000 ng·mL~(-1)的浓度范围内线性较好(r=0.997 82,n=7),高、中、低浓度日内及日间精密度均不高于13.63%,准确度在102.26%~108.95%内,提取回收率为92.36%,96.06%,100.71%。讨论本方法简单,且灵敏度高、特异性好,可用于人血清以及脑脊液中青霉素G浓度测定以及为血清与脑脊液中青霉素浓度相关性研究提供平台。
OBJECTIVE To establish a HPLC-MS/MS method for determination of penicillin in human serum and cerebrospinal(CSF), which can be used to determine the concentration of penicillin in the cerebrospinal fluid and serum of patients with neurosyphilis. METHODS Penicillin G-d7 was employed as the internal standard.Agilent ZORBAX Eclipse XDB-C_(18)(4.6 mm×50 mm, 1.8 μm) column was used to separate the analytes, and the mobile phase was methanol-water(82.5∶17.5, containing 3.5 mmol·L~(-1) ammonium formate) at a flow rate of 0.5 mL·min~(-1).Determination of penicillin G in serum and CSF were performed with multiple reaction monitoring(MRM) using positive electrospray ionization by triple quadrupole mass spectrometer. RESULTS In serum, calibration curves for penicillin had great linearity(r=0.999 1, n=7) within the range of 50-5 000 ng·mL~(-1).The inter-and intra-day precisions of high, medium and low concentrations were not more than 11.26% and accuracies were between 98.65% and 103.46% while the extraction recoveries were 99.64%, 101.21% and 105.22%, respectively.In CSF, calibration curves for penicillin had good linearity(r=0.997 82, n=7)within the range of 10-1 000 ng·mL~(-1).The inter-and intra-day precisions of high, medium and low concentration were not more than 13.63% and accuracies was between 102.26% and 108.95% while the extraction recoveries were 92.36%, 96.06% and 100.71%. CONCLUSION The current method is simple, sensitive, specific, and can be used to the determination of penicillin concentration in human serum as well as cerebrospinal fluid and the correlation studies between serum and cerebrospinal fluid penicillin concentrations.

关键词(KeyWords): 高效液相色谱串联质谱法;脑脊液;血清;青霉素G;治疗药物监测
HPLC-MS/MS;cerebrospinal fluid;serum;penicillin;therapeutic drug monitoring

Abstract:

Keywords:

基金项目(Foundation): 广东省卫生计生适宜推广项目(粤卫办函[2018]326号);; 广东省医学科学技术研究基金项目(A2020214);; 广东省医院药学研究基金(2021A11)

作者(Author): 董琳;卢浩扬;邱萍英;温预关;
DONG Lin;LU Haoyang;QIU Pingying;WEN Yuguan;Pharmaceutical Department,The Affiliated Brain Hospital of Guangzhou Medical University,Guangzhou Huiai Hospital,Guangdong Engineering Technology Research Center for Translational Medicine of Mental Disorders;Hunan Agricultural University;Clinical Laboratory,The Affiliated Brain Hospital of Guangzhou Medical University,Guangzhou Huiai Hospital,Guangdong Engineering Technology Research Center for Translational Medicine of Mental Disorders;

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