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柱前衍生HPLC-UV法测定氯氮平片中乳糖的含量
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国家自然科学基金资助项目（21705044，21804040）；湖南省自然科学基金资助项目（2019JJ50134）；湖南省 教育厅科学研究基金资助项目（19C0554）；化学生物传感与计量学国家重点实验室开放课题基金资助项目 （2018015）；湖南工业大学“绿色包装与安全”专项研究基金资助项目（2017ZBLY14）


Determination of Lactose in Clozapine by Pre-Column Derivatization HPLC-UV
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    摘要:

    采用1-苯基-3-甲基-5-吡唑啉酮（PMP）为衍生试剂，建立柱前衍生高效液相色谱法准确测定氯氮平片中乳糖的含量。实验结果显示，在0.060 4~0.399 7 mg/mL范围内，衍生目标物的峰面积与乳糖质量浓度呈现良好的线性关系，线性相关系数R2为0.999 4，加标回收率在96.7%~99.2%之间，定量限为0.32 μg/mL。随机抽选3个批次氯氮平片仿制样品进行检测，乳糖含量分别是42.09, 43.36, 43.45 mg/片，实测含量与处方含量的偏差不超过2.0 mg/片，结果完全满足氯氮平参比制剂中乳糖含量的检测需要。与现有的检测方法相比较，所提方法具有专属性强、灵敏度高、结果准确可靠等优点，可为氯氮平一致性评价处方的开发提供数据支持，有利于加快仿制药的开发速率和成功率。

    Abstract:

    A high-performance liquid chromatography (HPLC) method based on 1-phenyl-3-methyl-5-pyrazolinone (PMP) as an agent of pre-derivatization was developed for the accurate determination of lactose content in clozapine tablets. The results showed that a good linear relationship between the peak area of the derivative product and lactose concentration was observed in the range of 0.060 4~0.399 7 mg/mL, the linear correlation coefficient R2 was 0.999 4. The recovery was within the range of 96.7%~99.2% and the limit of quantification was estimated to be 0.32 μg/mL. Three batches of clozapine tablet imitation samples were randomly selected for testing, and the lactose contents were 42.09 mg/tablet, 43.36 mg/tablet and 43.45 mg/tablet, respectively. The deviation between the measured results and the prescribed content was less than 2.0 mg/ tablet, and the results could fully meet the requirement of detection of lactose in drugs. Moreover, compared with the existing tests, this method had the advantages of high specificity, high sensitivity, accurate and reliable results, and could provide data support for the development of clozapine consistency evaluation prescription, which is beneficial to the acceleration in the development and success rate of generic drugs.

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陈 瑶,汤建新,唐 英.柱前衍生HPLC-UV法测定氯氮平片中乳糖的含量[J].包装学报,2021,13(4):16-23.

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  • 收稿日期:2021-03-21
  • 在线发布日期: 2021-09-16
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