| 引用本文: | 莫霞,尚德为,倪晓佳,张明,温预关,程国华.LC-MS/MS测定人尿液中伪麻黄碱含量[J].中国现代应用药学,2015,32(4):467-471. |
| MO Xia,SHANG Dewei,NI Xiaojia,ZHANG Ming,WEN Yuguan,CHENG Guohua.Determination of Pseudoephedrine in Urine by LC-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2015,32(4):467-471. |
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| 摘要: |
| 目的 建立测定人尿液中伪麻黄碱药物浓度的方法。方法 采用LC-MS/MS进行测定。色谱柱：美国 Agilent Eclipse plus C18(4.6 mm×100 mm，3.5 μm)；流动相：甲醇-水(3︰1，含0.005 mol?L-1甲酸铵和0.1%甲酸)；流速：0.5 mL?min-1；柱温：40 ℃。质谱条件：电喷雾电离源(ESI)，正离子化，扫描方式为选择性离子监测，伪麻黄碱m/z 166.2→148.1，内标对乙酰氨基酚m/z 152.1→110.1。结果 尿液中伪麻黄碱浓度在500~300 000 μg?L-1(r2=0.998)内呈良好的线性关系，其批内、批间精密度RSD分别≤4.41%与≤10.04%；伪麻黄碱和内标的提取回收率均>90%；尿液中伪麻黄碱的平均累积排泄率为44.57%。结论 本研究建立的LC-MS/MS测定人尿液中伪麻黄碱的方法准确、简便、灵敏、重复性好，可用于临床研究中伪麻黄碱的尿药含量测定。 |
| 关键词: 液相色谱-质谱法 伪麻黄碱 尿液 |
| DOI： |
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| 基金项目:广东省自然科学基金(8151037001000001) |
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| Determination of Pseudoephedrine in Urine by LC-MS/MS |
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MO Xia1,2, SHANG Dewei3, NI Xiaojia3, ZHANG Ming3, WEN Yuguan3, CHENG Guohua1
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1.Pharmacy College of Jinan University, Guangzhou 510632, China;2.Guangdong Women and Children’s Hospital, Guangzhou 510000, China;3.Guangzhou Huiai Hospital, Guangzhou 510520, China
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| Abstract: |
| OBJECTIVE To establish a method for determination of pseudoephedrine in urine samples of healthy volunteers. METHODS The pseudoephedrine was determined by LC-MS/MS. The separation was carried on an Agilent Eclipse plus C18(4.6 mm×100 mm, 3.5 μm) colume with a mobile phase of methanol-0.005 mol?L-1 ammonium formate apueous solution with 0.1% formic acid (3∶1) at the flow rate of 0.5 mL?min-1, The column formate temperature was set at 40 ℃. ESI source was applied and operated in positive ion mode. Quantitative determination was performed by using selective reaction monitoring (SRM) of m/z 166.2→148.1 for pseudoephedrine and m/z 152.1→110.1 for paracetamol used as internal standard. RESULTS Pseudoephedrine in urine samples showed good linearity in the range of 500?300 000 μg?L-1(r2=0.998). The intra-batch and inter-batch precisions(RSD) were ≤4.41% and ≤10.04%, respectively. The extraction recoveries of pseudoe- phedrine and internal standard were more than 90%. The average cumulative excretion of pseudoephedrine in urine was 44.57%. CONCLUSION The method that using LC-MS/MS to determine pseudoephedrine in urine is accurate, simple and sentitive, and it has a good reproducibility. This method can be applied to the clinical pharmacokinetic study and therapeutic drug monitoring of pseudoephedrine. |
| Key words: LC-MS/MS pseudoephedrine urine |
