| 摘要: |
| 目的：建立高效液相色谱（HPLC）同时测定肺力咳合剂中苯甲酸钠等6种防腐剂含量的方法。方法：采用HPLC，色谱柱为Agilent XDB-C18色谱柱（250 mm×4.6 mm，5 μm），流动相：甲醇-0.025 mol/L磷酸二氢钠溶液（梯度洗脱）；流速：1.0 mL/min；柱温30 ℃，检测波长228 nm、255 nm。结果：肺力咳合剂中苯甲酸钠在0.063 54～211.800 00 μg（r=0.999 9）、山梨酸钾在0.066 06～220.200 00 μg（r=0.999 9）、对羟基苯甲酸甲酯在0.062 70～209.000 00 μg（r=0.999 9）、对羟基苯甲酸乙酯在0.066 12～220.400 00 μg（r=0.999 9）、对羟基苯甲酸丙酯在0.067 98～226.600 00 μg（r=0.999 9），对羟基苯甲酸丁酯在0.063 30～211.000 00 μg（r=0.999 9）范围内线性良好，平均回收率分别为100.72%（RSD=0.82%）、104.82%（RSD=1.59%）、101.11%（RSD=0.25%）、102.39%（RSD=1.33%）、102.56%（RSD=1.35%）、101.09%（RSD=0.34%）。10批样品中均未检出山梨酸钾、对羟基苯甲酸甲酯、对羟基苯甲酸丁酯，苯甲酸钠、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯的含量分别为2.132 6~2.602 6 mg/mL、0.110 8~0.126 0 mg/mL、0.399 9~0.408 9 mg/mL。结论：该方法具有操作简单，专属性强，准确度高的优点，可以更全面的控制肺力咳合剂中防腐剂的含量。 |
| 关键词: 肺力咳合剂 苯甲酸钠 山梨酸钾 对羟基苯甲酸甲酯 对羟基苯甲酸乙酯 对羟基苯甲酸丙酯 对羟基苯甲酸丁酯 含量测定 高效液相色谱法 |
| DOI：doi:10.13407/j.cnki.jpp.1672-108X.2022.09.007 |
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| 基金项目: |
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| Simultaneous Determination of 6 Kinds of Preservatives Including Sodium Benzoate in Feilike Mixture by High Performance Liquid Chromatography |
| Tang Chuan, Shen Xuebin, Gui Ling |
| (The People’s Hospital of Chizhou, Anhui Chizhou 247000, China) |
| Abstract: |
| Objective: To establish the method for simultaneous determination of 6 preservatives including sodium benzoate in Feilike mixture by high performance liquid chromatography (HPLC). Methods: HPLC was performed on Agilent XDB-C18 column (250 mm×4.6 mm, 5 μm) with mobile phase of methanol-0.025 mol/L sodium dihydrogen phosphate solution (gradient elution). The flow rate was 1.0 mL/min. The column temperature was 30 ℃, and the detection wavelength was 228 nm and 255 nm. Results: There were good linearity in the range from 0.063,54 to 211.800,00 μg (r=0.999,9) for sodium benzoate, from 0.066,06 to 220.200,00 μg (r=0.999,9) for potassium sorbate, from 0.062,70 to 209.000,00 μg (r=0.999,9) for methyl p-hydroxybenzoate, from 0.0661,2 to 220.400,00 μg (r=0.999,9) for ethyl p-hydroxybenzoate, from 0.067,98 to 226.600,00 μg (r=0.999,9) for propyl p-hydroxybenzoate, from 0.063,30 to 211.000,00 μg (r=0.999,9) for butyl p-hydroxybenzoate. The average recoveries were 100.72% (RSD=0.82%), 104.82% (RSD=1.59%), 101.11% (RSD=0.25%), 102.39% (RSD=1.33%), 102.56% (RSD=1.35%) and 101.09% (RSD=0.34%), respectively. Sodium benzoate, methyl p-hydroxybenzoate and butyl p-hydroxybenzoate were not detected in 10 batches of samples, and the contents of sodium benzoate, ethyl p-hydroxybenzoate and propyl p-hydroxybenzoate were respectively from 2.132,6 to 2.602 6 mg/mL, from 0.110,8 to 0.126,0 mg/mL, from 0.399,9 to 0.408,9 mg/mL. Conclusion: The method has the advantages of simple operation, strong specificity and high accuracy, and can comprehensively control the content of preservatives in Feilike mixture. |
| Key words: Feilike mixture sodium benzoate potassium sorbate methyl p-hydroxybenzoate ethyl p-hydroxybenzoate propyl p-hydroxybenzoate butyl p-hydroxybenzoate content determination high performance liquid chromatography |
