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麦味地黄口服液防腐剂及溶剂残留量研究

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目的 建立麦味地黄口服液中防腐剂(苯甲酸、山梨酸)及溶剂残留量(甲醇、乙醇)的检查和评价方法,为麦味地黄口服液质量安全评价提供技术支持。方法 甲醇和乙醇残留量的检查采用6%(V/V)氰丙基苯基-94%(V/V)二甲基聚硅氧烷(DB-624)为固定液的毛细管柱(30 m×0。32 mm×1。8μm);程序升温;进样口温度为200℃;FID检测器温度为250℃;载气氮气流速为2。0 mL/min;顶空分流进样,分流比20∶1。苯甲酸和山梨酸的检测采用Agilent Eclipse XDB-C18色谱柱(250 mm×4。6 mm,5μm);以乙腈-0。1% 磷酸溶液为流动相,梯度洗脱;流速1。0 mL/min;苯甲酸和山梨酸检测波长分别为230 nm、260 nm;柱温30℃。结果 建立的方法线性、专属性、稳定性、重复性良好。对6家企业生产的15批次麦味地黄口服液进行检测,结果有1家企业的3批次样品乙醇残留量超标。结论 所建立的方法准确、专属性强,此方法可用于麦味地黄口服液的质量安全评价。
Study on the Preservative and Solvent Residues of Maiwei Dihuang Oral Liquid
Objective To establish a method for the detection and evaluation of preservatives (benzoic acid and sorbic acid) and solvent residues (methanol and ethanol) in maiwei dihuang oral liquid,and to provide technical support for the quality safety evaluation of maiwei dihuang oral liquid. Methods Determination of residual methanol and ethanol using a capillary column (30 m × 0.32 mm×1.8 μm) with 6% (V/V) cyanopropyl phenyl-94% (V/V) dimethylpolysiloxane (DB-624) as fixed liquid;with a programmed temperature increase;the inlet temperature was 200 ℃;the FID detector temperature was 250 ℃;the carrier gas flow rate was 2.0 mL/min;and the split ratio was 20∶1. The detection of benzoic acid and sorbic acid was performed using an Agilent Eclipse XDB-C18 column (250 mm × 4.6 mm,5 μm);the mobile phase was a mixture of acetonitrile and 0.1% phosphoric acid;the flow rate was 1.0 mL/min;the detection wavelengths for benzoic acid and sorbic acid were 230 nm and 260 nm,respectively;and the column temperature was 30 ℃ . Results The established method has good linearity,specificity,stability,and reproducibility.The results of the detection of 15 batches of maiwei dihuang oral liquid produced by 6 enterprises showed that 3 batches of one enterprise had excessive ethanol residues. Conclusion The established method is accurate and specific,and this method can be used for the quality safety evaluation of maiwei dihuang oral liquid.

Maiwei dihuang oral liquidHeadspace-gas chromatographyResidual solventLiquid chromatographyBenzoic acidSorbic acid

梅赞、段玮、于潜、梁基琳

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吉安市食品药品检验检测中心,江西吉安 343000

麦味地黄口服液 顶空-气相色谱 溶剂残留 液相色谱 苯甲酸 山梨酸

2024

药品评价
江西省药学会

药品评价

影响因子:0.672
ISSN:1672-2809
年,卷(期):2024.21(8)