[1]郭进艳,孙文利,刘红星,等.高效液相色谱-串联质谱法测定血液病患者血液甲泼尼龙浓度的应用[J].现代检验医学杂志,2024,39(06):211-217.[doi:10.3969/j.issn.1671-7414.2024.06.037]
　GUO Jinyan,SUN Wenli,LIU Hongxing,et al.Application of HPLC-MS/MS in the Determination of Methylprednisolone Concentration in Patients with Hematological Diseases[J].Journal of Modern Laboratory Medicine,2024,39(06):211-217.[doi:10.3969/j.issn.1671-7414.2024.06.037]
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高效液相色谱-串联质谱法测定血液病患者血液甲泼尼龙浓度的应用()
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《现代检验医学杂志》[ISSN:/CN:]

卷:
第39卷
期数:
2024年06期
页码:
211-217
栏目:
论著
出版日期:
2024-11-15

文章信息/Info

Title:
Application of HPLC-MS/MS in the Determination of Methylprednisolone Concentration in Patients with Hematological Diseases
文章编号:
1671-7414（2024）06-211-07
作者:
郭进艳; 孙文利; 刘红星; 王 磊
（河北燕达陆道培医院检验医学科，河北廊坊 065201）
Author(s):
GUO Jinyan;  SUN Wenli;  LIU Hongxing;  WANG Lei
（Department of Laboratory Medicine, Hebei Yanda Ludaopei Hospital, Heibei Langfang 065201, China）
关键词:
甲泼尼龙; 高效液相色谱- 串联质谱; 治疗药物监测
分类号:
R552；Q503
DOI:
10.3969/j.issn.1671-7414.2024.06.037
文献标志码:
A
摘要:
目的 建立高效液相色谱- 串联质谱法（HPLC-MS/MS）测定血液病患者血浆甲泼尼龙浓度，并应用于指导临床合理用药。方法 以甲泼尼龙-d3 为内标，甲醇沉淀血浆蛋白和萃取甲泼尼龙。月旭Ultimate XB-C18 柱[4.6mm ×50mm，5μm）为色谱柱，流动相为含0.1%(v/v) 甲酸的甲醇溶液（1 ∶ 1 000）- 水溶液[ 含0.1% (v/v) 甲酸+2 mmol/L乙酸铵]，流速0.8 ml/min，柱温60℃，进样量5μl。采用电喷雾离子源，正离子模式下进行多反应监测，同时监测甲泼尼龙质荷比（m/z） 375. 4 → 339.4（定性离子），甲泼尼龙 m/z 375. 4 → 357. 3 ( 定量离子)，甲泼尼龙-d3 m/z 378.2 → 360. 3。以甲泼尼龙和甲泼尼龙-d3 峰面积比为定量依据，计算血浆甲泼尼龙浓度，并评价其性能。结果 甲泼尼龙在10 ～ 1 000ng/ml 范围线性关系良好（r2 = 0.996 7），定量下限为10ng/ml ；日内、日间精密度实验结果相对标准差（RSD）均小于15%；提取回收率为99.52% ～ 104.79%；甲泼尼龙样品在经历3 次反复冻融（﹣ 20℃～室温）循环条件下稳定，处理后的样品在室温、4℃环境中放置24h 均稳定（RSD <15%）。16 例患者甲泼尼龙血药浓度在0 ～ 258ng/ml 范围内。结论 该方法可准确、快速、简便地检测甲泼尼龙浓度，适用于临床甲泼尼龙血药浓度检测。
Abstract:
Objective To establish a high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method for determining the plasma concentration of methylprednisolone in patients with hematological diseases, and apply it to guide the clinical application. Methods Plasma samples were subjected to methanol-precipitated protein containing internal standard methylprednisolone-d3. The HPLC system was equipped with an Ultimate XB-C18 (4.6mm×50mm, 5 μm particle size), maintained at 60℃ , and 5 μl of the supernatant was injected. Mobile phases consisting of 0.1% (v/v) formic acid (1∶1 000) and 2 mmol/L ammonium acetate in water (B) and 0.1% (v/v) formic acid(1∶1 000) in methanol at a flow rate of 0.8 ml/ min was used. The electrospray ionization (ESI) source was operating in positive ion mode. Multiple reaction monitoring (MRM) was applied for the detection of the components：Methylprednisolone mass-to-charge ratio (m/z) 375.4 → 339.4 (qualitative ions), methylprednisolone m/z 375.4 → 357.3 (quantitative ions), methylprednisolone-d3 m/z 378.2 → 360.3. The peak area ratio of methylprednisolone to methylprednisolone-d3 was used as the quantitative basis. The concentration of methylprednisolone in plasma was calculated and its performance was investigated. Results The linear range of methylprednisolone was 10~1 000ng/ml (r2 = 0.996 7), and the lower limit of quantification was 10 ng/ml. The RSDs of intra-day and inter-day precision results were less than 15% and the relative recovery ranged from 99.52% ～ 104.79%. For methylprednisolone, the samples were stable at -20 ℃ after three repeated freeze-thaw cycles. The prepared samples were stable at room temperature and 4 ℃ for 24h (RSDs <15%). The steady-state blood drug concentrations of methylprednisolone in 16 patients were in the ranges of 1 ～ 258 ng/ml. Conclusion The HPLC-MS/MS method can accurately, rapidly and simply detect the concentration of methylprednisolone， and be suitable for clinical application.

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备注/Memo

备注/Memo:
基金项目：河北省卫生健康委医学科学研究课题 （编号：20210319）。
作者简介：郭进艳（1995-），女，本科，初级药师，研究方向：血药浓度监测及药学研究，E-mail: 1281216267@qq.com。
通讯作者：王 磊（1984-），男，硕士，主管药师，研究方向：血药浓度监测及医院药学研究，E-mail:rosie1982@163.com。
更新日期/Last Update: 2024-11-15