Objective: To establish a method for the determination of nimesulide in human plasma, organize external quality assessment, evaluate the determination capacity of pharmacokinetic laboratories and discuss the process of external quality assessment in this field and the method of result evaluation. Methods: An HPLC- MS/MS analysis method was adopted. The analysis was performed on a Xbridge C18 column(2.1 mm×50 mm, 3.5 μm), using acetonitrile-0.1% formic acidas the mobile phase with gradient elution.The flow rate was 0.45 mL·min-1 and the column temperature was 40 ℃ .Negative electrospray ion source (ESI) and multiple reaction monitoring (MRM) mode were used. The MS /MS ion transitions monitored were m/z 307.1→229.0 and m/z 296.0→204.7 for nimesulide and internal stan dardhydrochlorothiazide, respectively.The homogeneity and stability of the test samples were prepared and evaluated according to the evaluation guidelines of China National Accreditation Service for Conformity Assessment and related guidelines. All results replied from participated laboratories were statistically analyzed. Results: The validation results meet the requirements of the drug concentration determination. The homogeneity and stability of quality evaluation samples meet the requirements of distribution and determination. The satisfaction rate of the laboratory returning results was 83.3% of the 18 participated laboratories. Conclusion: This external quality assessment activity evaluated the report results of 18 laboratories and analyzed the influencing factors of the system, which provided a basis for biological sample testing laboratories to find problems in their own detection, monitor and improve laboratory capabilities. It also provides help for expanding the scope of external quality assessment activities, continuing to organize and implement, and establishing a long-term mechanism for laboratory capability verification.
LIU Yuan, YANG Yan-yan, LI Yang, ZHAO Shi-jing, YANG ming, SHI Ain-xin
. Determination of nimesulideconcentration in human plasma by HPLC-MS/MS and its application in external quality assessment*[J]. Chinese Journal of Pharmaceutical Analysis, 2022
, 42(6)
: 1029
-1036
.
DOI: 10.16155/j.0254-1793.2022.06.15
[1] KRLEZA JL, CELAP I, TANASKOVIC JV. External quality assessment in croatia: problems, challenges, and specific circumstan ces[J].Biochem Med (Zagreb), 2017, 27(1):86
[2] MILLER WG, JONES GR, HOROWITZ GL, et al. Proficiency testing/external quality assessment: current challenges and future directions[J].Clin Chem, 2011, 57(12):1670
[3] KÜÇÜkgÜzel ZEL SG, KÜÇÜkgÜzel ZEL I, ORAL B, et al. Detection of nimesulide metabolites in rat plasma and hepatic subcellular fractions by HPLC-UV/DAD and LC-MS/MS studies[J].Eur J Drug Metab Pharmacokinet, 2005, 30(1-2):127
[4] SENNA GE, PASSALACQUA G, ANDRI G, et al. Nimesulide in the treatment of patients intolerant of aspirin and other NSAIDs[J].Drug Saf, 1996, 14(2):94
[5] SUN X, XUE KL, JIAO XY, et al. Simultan eous determination of nimesulide and its four possible metabolites in human plasma by LC-MS/MS and its application in a study of pharmacokinetics[J].J Chromatogr B Anal Technol Biomed Life Sci, 2016, 1027:139
[6] HALDER D, DAN S, SARKAR P, et al. LC-MS/MS determination of 4-hydroxynimesulide, an active metabolite of nimesulide and application to bioequivalence study in Indian subjects[J].Eur J Mass Spectrom (Chichester), 2019, 25(5):399
[7] 刘炜,李晓晔,程维明.LC-MS/MS法测定人血浆中尼美舒利的浓度[J].中国药房, 2010, 21(2):2
LIU W, LI XY, CHENG WM. Dtermination of nimesulide in human plasma by LC-MS[J].J China Pharm, 2010, 21(2):2
[8] 陈沫, 卢永翎, 杭太俊,等. 尼美舒利分散片在健康人体内的药代动力学及生物等效性的 LC-MS/MS研究[J].药物分析杂志, 2013, 33(1):30
CHEN M, LU YL, HANG TJ, et al. Clinical pharmacokinetics and bioequivalence of nimesulide dispersible tablets by LC-MS/MS method[J].Chin J Pharm Anal, 2013, 33(1):30
[9] 闫颖, 张顺利, 钟堃,等. 2010~2012年度治疗药物监测室间质评结果分析[J].中国药物警戒, 2013, 10(12):755
YAN Y, ZHANG SL, ZHONG K, et al. Analysis of external quality assessment results for therapeutic drug monitoring from 2010 to 2012[J].J Pharmacovigil, 2013, 10(12):755
[10] 赵新玥, 赵文, 陈华. pH测定检验能力验证及评价新方法的应用[J].药物分析杂志, 2018, 38(3):545
ZHAO XY ZHAO W CHEN H. Application of new methods to the proficiency testing project of pH determination and its evaluation[J].Chin J Pharm Anal, 2018, 38(3):545
[11] 中华人民共和国药典 2020 年版.四部[S].2020: 50
ChP 2020. Vol Ⅳ[S].2020: 50
[12] CNAS GL03 能力验证样品均匀性和稳定性评价指南[S].2015
CNAS GL03Guidance on Evaluating the Homogeneity and Stability of Samples Used for Proficiency Testing[S].2015
[13] CNAS GL002 能力验证结果的统计处理和能力评价指南[S].2018
CNAS GL002Guidance on Statistic Treatment of Proficiency Testing Results and Performance Evaluation[S].2018
[14] BS ISO 13528-2005 Statistical methods for use in proficiency testing by interlaboratory comparisons[S].2005
