Cooling crystallization of paracetamol in ethanol solution based on real-time ATR-UV measurement

GUAN Guoqiang; TANG Kai; LI Hong; LU Shuaitao; JIANG Yanbin

doi:10.11949/j.issn.0438-1157.20150763

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Cooling crystallization of paracetamol in ethanol solution based on real-time ATR-UV measurement

更新时间：2025-12-10

- Cooling crystallization of paracetamol in ethanol solution based on real-time ATR-UV measurement
- CIESC Journal Issue 9, Pages: 3580-3587(2015)
- 作者机构：
  
  1. 华南理工大学化学与化工学院,广东,广州,510640
  2. 传热强化与过程节能教育部重点实验室,广东,广州,510640
  3. 广东肇庆星湖生物科技股份有限公司技术中心,广东,肇庆,526040
- 作者简介：
- 基金信息：
- DOI：10.11949/j.issn.0438-1157.20150763
  CLC： Q420.6+1
- Online First：05 September 2015，
  
  Published：05 September 2015
- 稿件说明：
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GUAN Guoqiang, TANG Kai, LI Hong, et al. Cooling crystallization of paracetamol in ethanol solution based on real-time ATR-UV measurement[J]. CIESC Journal, 2015, (9): 3580-3587.
DOI：

GUAN Guoqiang, TANG Kai, LI Hong, et al. Cooling crystallization of paracetamol in ethanol solution based on real-time ATR-UV measurement[J]. CIESC Journal, 2015, (9): 3580-3587. DOI： 10.11949/j.issn.0438-1157.20150763.

摘要

以无水乙醇-扑热息痛为模型物体系

对基于衰减全反射紫外光谱(ATR-UV)分析的结晶过程实时浓度检测进行了研究。采用偏最小二乘法进行结晶过程浓度关联

建立了ATR-UV实时浓度检测模型

该模型实时分析结果与重量法测量结果一致

均方根平均偏差为0.0075。通过ATR-UV实时浓度分析关联结晶过程的过饱和度变化

并结合聚焦光束反射测量技术分析了不同降温方式对结晶产品的影响。结果表明:相对于自然冷却和线性冷却温度控制方式

受控冷却过程能获得尺寸更大、分布更均一的晶体产品。

Abstract

Real-time concentration determination is critical in process analytical technology for advance quality control of crystallization. A novel approach is presented to correlate in-situ concentration of paracetamol in ethanol solution with the attenuated total reflection/ultraviolet (ATR-UV) spectrum by using the partial least squares method. The correlated concentrations are well consistent with the measurement of gravimetric method and the root-mean-square derivation is found to be 0.0075. Supersaturation correlation based on the developed ATR-UV in-situ concentration measurement

coupled with focused beam reflection measurement for monitoring the nucleation and growth during crystallization procedure

is utilized to investigate the effect of three cooling policies on cooling crystallization

i.e.

natural cooling policy (NCP)

linear cooling policy (LCP) and control cooling policy (CCP). The results show that the CCP has advantages over NCP and LCP in producing more crystals with the large and well-distributed crystal sizes.

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