CN113686807A - 一种快速检测2-氯-1-（4-异丁基苯）丙酮含量的方法 - Google Patents
一种快速检测2-氯-1-（4-异丁基苯）丙酮含量的方法 Download PDFInfo
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Abstract
本发明提供了一种快速检测2‑氯‑1‑(4‑异丁基苯)丙酮含量的方法，先通过测定不同含量的2‑氯‑1‑(4‑异丁基苯)丙酮溶液的近红外吸收光谱；在相同的光谱测量条件下测定已知含量2‑氯‑1‑(4‑异丁基苯)丙酮溶液的验证样品得到2‑氯‑1‑(4‑异丁基苯)丙酮含量预测值，分析预测值与已知含量参考值得到二者的相关性图，然后通过相关性图快速检测2‑氯‑1‑(4‑异丁基苯)丙酮的含量；本发明解决了布洛芬生产过程中对中间体2‑氯‑1‑(4‑异丁基苯)丙酮传统检测方法烦琐、耗时等问题。
Description
技术领域
本发明属于化学分析技术领域，涉及一种快速检测2-氯-1-(4-异丁基苯)丙酮含量的方法。
技术背景
2-氯-1-(4-异丁基苯)丙酮，分子式C13H17ClO，易溶于二氯甲烷、石油醚等有机溶剂，该产品是生产非甾体消炎药布洛芬的主要中间体。2-氯-1-(4-异丁基苯)丙酮的主流合成路线是以异丁苯、氯代丙酰氯为原料，经傅克酰基化反应制得，该中间体再经过缩合、转位重排、水解、酸化等反应可生成布洛芬。
目前生产中对2-氯-1-(4-异丁基苯)丙酮的含量检测方法主要有气相面积归一化法、液相内标法，但是这两种方法配样步骤相对繁琐，主成分峰保留时间长，每检测一次大约需要40-60分钟，严重制约布洛芬产能的提升。因此，探寻一种简便、快速检测2-氯-1-(4-异丁基苯)丙酮含量的方法势在必行。
近红外光谱分析技术作为一种现代分析技术，具有简便、快速、不破坏样品结构、能够实现在线分析等特点，已被应用于医药、化工中间体的含量检测中。因此，本发明采用近红外光谱分析技术，建立一种快速检测2-氯-1-(4-异丁基苯)丙酮含量的方法。
发明内容
本发明提供了一种快速检测2-氯-1-(4-异丁基苯)丙酮含量的方法，包括如下步骤：
(1)准备一系列已知含量的2-氯-1-(4-异丁基苯)丙酮溶液；
(2)将已知含量的2-氯-1-(4-异丁基苯)丙酮溶液进行近红外吸收光谱扫描；
(3)对所得近红外光谱光学数据进行基线校正Baseline Correction和光程校正Thickness Correction；
(4)利用化学计量学分析软件Unscrambler进行偏最小二乘回归分析(PLS)，得近红外定量分析模型；
(5)在相同的光谱测量条件下测定已知含量2-氯-1-(4-异丁基苯)丙酮溶液的验证样品，经定量分析模型计算得到2-氯-1-(4-异丁基苯)丙酮含量预测值。
分析预测值与已知含量参考值的相关性。
所述准备一系列已知含量的2-氯-1-(4-异丁基苯)丙酮溶液为36份，含量范围为91.81-96.55％(g/ml)。
所述将已知含量的2-氯-1-(4-异丁基苯)丙酮溶液进行近红外吸收光谱扫描，波长范围为9300-4700cm-1，分辨率为16cm-1，扫描次数：64次，测量温度为18-25℃，每份样品扫描3次，保存平均光谱。
本发明解决了布洛芬生产过程中对中间体2-氯-1-(4-异丁基苯)丙酮传统检测方法烦琐、耗时等问题。
附图说明
图1为不同含量的2-氯-1-(4-异丁基苯)丙酮溶液近红外吸收光谱；
图2为2-氯-1-(4-异丁基苯)丙酮溶液含量的参考值与预测值的相关性图。
具体实施方式
为使本发明的目的、技术方案及效果更加清楚、明确，以下将配合实施例来对本发明进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明。
实施例1
1、准备36份不同含量的2-氯-1-(4-异丁基苯)丙酮溶液，含量范围为91.81-96.55％(g/ml)，保证此含量范围能够覆盖生产中2-氯-1-(4-异丁基苯)丙酮溶液含量范围(92-96％，g/ml)具体数据见表1：
表1:36份2-氯-1-(4-异丁基苯)丙酮溶液含量数据。
2、用ABB公司MB3600型近红外光谱分析仪,将36份已知含量的2-氯-1-(4-异丁基苯)丙酮溶液分别进行近红外光谱测定，以空气为参比，设置扫描波长范围为：9300-4700cm-1，分辨率：16cm-1，扫描次数：64次，每个样品重复测定3次，求平均光谱。所得不同含量2-氯-1-(4-异丁基苯)丙酮溶液的近红外吸收光谱如图1所示。
3、对所得近红外光谱光学数据进行基线校正Baseline Correction和光程校正Thickness Correction。
4、利用化学计量学分析软件Unscrambler进行偏最小二乘回归分析(PLS)，所得近红外定量分析模型的决定系数(R2)为0.9217，交互验证均方根误差(RMSEC)为0.5093和预测均方根误差(RMSEP)为0.5909。
5、在相同的光谱测量条件下测定16份已知含量2-氯-1-(4-异丁基苯)丙酮溶液的验证样品，经定量分析模型计算得到2-氯-1-(4-异丁基苯)丙酮含量预测值。具体数值见表2，分析预测值与已知含量参考值得到图2所示的相关性图。从图2可以看出，应用本发明的方法，样品的2-氯-1-(4-异丁基苯)丙酮含量预测值与参考值之间具有很好的相关性，R为0.998，因此，可认定近红外的检测数据是准确可靠的，此方法能够实现快速检测2-氯-1-(4-异丁基苯)丙酮的含量。
表2:18份验证样品预测值和参考值数据。
| 序号 | 参考值 | 预测值 | 绝对偏差 |
| 1 | 91.84 | 91.79 | 0.05 |
| 2 | 92.57 | 92.60 | -0.03 |
| 3 | 93.37 | 93.27 | 0.10 |
| 4 | 94.34 | 94.40 | -0.06 |
| 5 | 94.45 | 94.50 | -0.05 |
| 6 | 94.94 | 95.05 | -0.11 |
| 7 | 94.90 | 95.10 | -0.20 |
| 8 | 95.42 | 95.46 | -0.03 |
| 9 | 95.53 | 95.58 | -0.04 |
| 10 | 96.05 | 95.90 | 0.15 |
| 11 | 95.70 | 95.83 | -0.13 |
| 12 | 95.84 | 95.86 | -0.02 |
| 13 | 95.84 | 95.90 | -0.06 |
| 14 | 95.94 | 96.03 | -0.08 |
| 15 | 96.20 | 96.15 | 0.06 |
| 16 | 96.29 | 96.31 | -0.02 |
Claims (3)
1.一种快速检测2-氯-1-(4-异丁基苯)丙酮含量的方法，其特征在于利用近红外光谱技术快速检测，包括以下步骤：
(1)准备一系列已知含量的2-氯-1-(4-异丁基苯)丙酮溶液；
(2)将已知含量的2-氯-1-(4-异丁基苯)丙酮溶液进行近红外吸收光谱扫描；
(3)对所得近红外光谱光学数据进行基线校正Baseline Correction和光程校正Thickness Correction；
(4)利用化学计量学分析软件Unscrambler进行偏最小二乘回归分析(PLS)，得近红外定量分析模型；
(5)在相同的光谱测量条件下测定已知含量2-氯-1-(4-异丁基苯)丙酮溶液的验证样品，经定量分析模型计算得到2-氯-1-(4-异丁基苯)丙酮含量预测值；分析预测值与已知含量参考值的相关性。
2.根据权利要求1所述的一种快速检测2-氯-1-(4-异丁基苯)丙酮含量的方法，其特征在于，所述步骤(1)中准备36份已知含量的2-氯-1-(4-异丁基苯)丙酮溶液，含量范围为91.81-96.55％(g/ml)。
3.根据权利要求1所述的一种快速检测2-氯-1-(4-异丁基苯)丙酮含量的方法，其特征在于，所述步骤(2)中用近红外光谱仪对已知含量的2-氯-1-(4-异丁基苯)丙酮溶液进行扫描，波长范围为9300-4700cm-1,分辨率为16cm-1，测量温度为18-25℃。
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| CN102323236A (zh) * | 2011-08-12 | 2012-01-18 | 山西振东制药股份有限公司 | 近红外光谱测定苦参提取过程多种成分含量的方法 |
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Application publication date: 20211123 |