| 摘要: |
| 目的 建立一种快速测定面膜中地塞米松含量的LC-MS法。方法 面膜样品加泼尼松为内标后，用饱和氯化钠和乙腈提取，用C18粉末净化后直接上机分析。测定采用SB-C18（50 mm×2.1 mm，1.8 μm）为分离色谱柱，以甲醇-0.1%甲酸（90∶10）为流动相，柱温35℃，流速0.2 mL·min-1，扫描方式是多反应监测模式。结果 地塞米松在0.2~10 μg·mL-1内线性良好（r=0.999 8），高中低水平的回收率分别为104.4%，95.8%和93.3%，相应RSD分别为1.0%，0.3%和1.1%。检测40批实际样品，检出1批地塞米松含量为3.51 mg·kg-1。结论 本方法可以快速准确地测定面膜中的地塞米松。 |
| 关键词: 地塞米松 内标 面膜 糖皮质激素 液质联用 |
| DOI：10.13748/j.cnki.issn1007-7693.2018.06.011 |
| 分类号:R917.101 |
| 基金项目: |
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| Fast Determination of Dexamethasone in Facial Mask by LC-MS |
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WANG Xincai1, HU Lei2
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1.Huzhou Institute for Food and Drug Control, Huzhou 313000, China;2.Zhejiang Institute for Food and Drug Control, Hangzhou 310052, China
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| Abstract: |
| OBJECTIVE To establish a fast liquid chromatography-mass spectrometry method for determination of dexamethasone in facial mask. METHODS The facial mask samples were added prednisone as internal standard, then extracted by saturated sodium chloride and acetonitrile, injected and analyzed after purified by C18 powder. An SB-C18 column (50 mm×2.1 mm, 1.8 μm) was used as stationary phase and methanol-0.1% formic acid (90:10) was used as the mobile phase. The flow rate was 0.2 mL·min-1 and the column temperature was 35℃. The scan mode was multi reaction monitoring. RESULTS The linear of dexamethasone acted well in range of 0.2-10 μg·mL-1(r=0.999 8). The recoveries of high, middle and low concentration were 104.4%, 95.8% and 93.3%, the RSDs were 1.0%, 0.3% and 1.1% respectively. There was one sample detected for 3.51 mg·kg-1dexamethasone in 40 actual samples. CONCLUSION This method has been validated for determination of dexamethasone in facial mask accurately and rapidly. |
| Key words: dexamethasone internal standard mask glucocorticoids LC-MS |
