| 王云霞,张苗苗,谢志民.变换波长高效液相色谱法测定茵栀黄口服液中防腐剂的含量[J].安徽医药,2022,26(5):877-881. |
| 变换波长高效液相色谱法测定茵栀黄口服液中防腐剂的含量 |
| Simultaneous determination of preservatives in Yinzhihuang oral liquid by HPLC with variable wavelength |
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| DOI：10.3969/j.issn.1009-6469.2022.05.007 |
| 中文关键词: 防腐剂，药物 苯甲酸 茵栀黄口服液 色谱法，高效液相 |
| 英文关键词: Preservatives,pharmaceutical Benzoic acid Yinzhihuang oral liquid Chromatography,high pressure liquid |
| 基金项目: |
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| 摘要点击次数: 956 |
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| 中文摘要: |
| 目的建立测定茵栀黄口服液中防腐剂的含量测定方法，并评价该制剂在防腐剂方面的安全性。方法采用高效液相色谱(HPLC)法。色谱柱为Agilent C18；流动相为甲醇-0.02 mol/L磷酸二氢钠溶液(用磷酸调pH值3.7)(V/V)，梯度洗脱；流速为1.0 mL/min；柱温为30 ℃；紫外检测器；苯甲酸以228 nm为检测波长，山梨酸和对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯以255 nm为检测波长。结果苯甲酸、山梨酸、对羟基苯甲酸甲酯(羟苯甲酯)、对羟基苯甲酸乙酯(羟苯乙酯)、对羟基苯甲酸丙酯(羟苯丙酯)、对羟基苯甲酸丁酯(羟苯丁酯)分别在进样量为77.11～4 935 ng(r=0.9999)、100.00～6 437 ng(r=0.999 9)、13.00～814 ng(r=0.999 9)、70.00～4 524 ng(r=0.999 9)、12.00～794 ng(r=0.999 9)、13.00～823ng(r=0.999 9)，峰面积积分值与进样量呈良好的线性关系；精密度(n=6)、重复性(n=6)、稳定性(24 h，n=8)试验的RSD均小于1.0%；最低方法检出限分别为0.600 ng、0.015 ng、0.025 ng、0.090 ng、0.010 ng、0.022 ng；最低方法定量限分别定为2.40 ng、0.14ng、0.33 ng、0.27 ng、0.04 ng、0.08 ng；加样回收率分别为100.69%、98.44%、101.21%、104.18%、103.95%、103.55%，RSD分别为0.24%、0.29%、0.72%、0.71%、0.44%、0.34%(n=6)。在32批样品中均未检测出除苯甲酸以外的其他防腐剂。结论该方法可用于茵栀黄口服液中防腐剂的定量分析；虽在抽检样品中未检测出其他防腐剂，为了提高其安全性，建议增订防腐剂检查项。 |
| 英文摘要: |
| Objective To establish a method for content determination of preservatives in Yinzhihuang oral liquid, and to evaluate the safety of the preservative.Methods High performance liquid chromatography (HPLC) with variable wavelength was used. The Agi-lent C18 (250 mm × 4.6 mm, 5 μm) column was used, methanol-0.02 mol/Lsodium dihydrogen phosphate solution (adjusting pH=3.7 byphosphate) was used as mobile phase in gradient elution mode at the flow rate of 1.0 mL/min, and the tempera-ture of column was 30 ℃.The analyte was determined with variable wavelength detector. Benzoic acid was detected at 228 nm, sorbic acid and methyl p-hydroxy-benzoate, ethylp-hydroxybenzoate, propyl p-hydroxybenzoate and butyl p-hydroxybenzoate were detected at 255 nm.Results The lin-ear ranges of benzoic acid, sorbic acid, methyl p-hydroxybenzoate, ethylp-hydroxybenzoate, propyl p-hydroxybenzoate and butyl p-hy-droxybenzoate were 77.11-4 935 ng (r=0.999 9), 100.00-6 437 ng (r=0.999 9), 13.00-814 ng (r=0.999 9), 70.00-4 524 ng (r=0.999 9),12.00-794 ng (r=0.999 9), 13.00-823 ng (r=0.999 9), respectively. RSDs of precision (n=6), reproducibility (n=6) and stability tests (24h, n=8) were all lower than 1.0%. The detection limits were 0.600 ng, 0.015 ng, 0.025 ng, 0.090 ng, 0.010 ng and 0.022 ng, respective-ly. The quantitation limits were 2.40 ng, 0.14 ng, 0.33 ng, 0.27 ng, 0.04 ng and 0.08 ng, respectively. The recoveries were 100.69%,98.44%, 101.21%, 104.18%, 103.95% and 103.55%. RSDs were 0.24%, 0.29%, 0.72%, 0.71%, 0.44% and 0.34% (n=6). Preserva-tives were not detected in addition to benzoic acid in 32 batches of samples.Conclusions This method is suitable for the determina-tion of preservatives in Yinzhihuang Oral liquid. Although the other preservatives were not detected in the sample, it is advisable to add the determination of preservatives so as to improve its safety. |
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