固态NMR Pharma解决方案

磁共振在多晶型的表征和定量中

尽管磁共振被认为是研究多晶型和无定形形式的公认的强大技术，但到目前为止，它属于很少的专家。然而，最近的技术进步使该技术能够将技术部署给更广泛的科学受众。通过引入台式光谱仪，我们已经克服了价格和复杂性障碍，并通过我们的高分辨率地板站立仪器大大提高了自动化和敏感性。

New benchtop NMR solutions

The minispec Form Check, is a benchtop spectrometer for the quantification of components in solids mixtures; such as a polymorph in the presence of another form; amorphous form in the presence of a polymorphs or a polymorph/amorphous forms in the presence of excipients. The minispec Form Check approaches the quantification of solid forms from a completely different angle to that of other techniques (PXRD, Raman, IR). It is a time-domain (TD) instrument, which means there is no fourier transform to carry out, and no frequency domain. The minispec Form Check pulls components apart based on their relaxation properties, - T1 relaxation in this case. The T1 relaxation time of a drug's crystalline and amorphous form is generally very different, making this technique ideal, especially for the quantification of low levels of amorphous form (LOQ < 1%), which is challenging by PXRD and is associated with a significant quantification error.

使开放式固态NMR成为现实的改进y

Although traditionally in the hands of few specialists, recent advances have enabled the deployment of the technique to the walk-up lab. Instruments are now equipped with the new iProbe, enabling automatic tuning and matching and magic angle adjustment; and sample changers driven by the same automation software used in liquid-state NMR.

IPROBE平台还包括液态探针和高分辨率魔术角旋转（HRMA）应用程序，可提供完整的自动化功能，以实现从一个样本更改为另一个样品时必要的调整和匹配步骤自动化。此外，这是solid-state NMR，还需要精确调整魔术角旋转位置。IPROBE CPMA具有使用KBR作为参考化合物的正确和精确选择正确方向的电动机。

The probe is currently offered at 400, 500 or 600 megahertz (MHz) base frequency for standard bore systems. It comes in a double channel set-up, meaning we have a proton channel which is also tunable to fluorine, and a broadband channel which goes from phosphorus down to nitrogen. Spinning speed, for four-millimeter samples, is up to 15-kHz magic-angle spinning.

The new "shuttle technology" enables the same sample changer to be used for both liquids and solids NMR, facilitating a simple upgrade from liquids to solids for half the price of a Powder X-ray Diffraction (PXRD) instrument!

用户利益：

• Identification and quantification of crystalline and amorphous content in APIs and formulated products
• 量化每种形式的数量而无需标准
  
• Multiple attribute: multiple nuclei can be analyzed, providing several unique spectra for each form
• Unique to NMR, relaxation times:
  

1. identify peaks for different crystalline forms, as each form’s relaxation time is usually unique
2. selectively enhance or remove different forms in a mixture of components, which can be useful for form identification and showing intellectual property infringement
3. predict both particle size and chemical degradation rates, especially in formulated products.

• Selectivity: labelling of nuclei such as¹³C和¹⁵N can be used to enhance certain signals when sensitivity is a challenge, and avoids peak overlap
  

CryoProbe for solids

The first ever cryogenically cooled probe forsolid-state NMR（CPMAS冷冻探针）对于分析非常少量的化合物特别有用，就像配方材料（药物）中多晶型/无定形形式一样。冷却的电子设备和冷却的探针设置，同时将样品本身保持在所需的实验温度下，使灵敏度提高了三到四倍，这转化为至少一个数量级生产率的顺序提高。

The probe is currently available in an HCN (proton, carbon, nitrogen) configuration for 600 MHz magnets and provides magic angle speeds of up to 20-KHz with 3.2 mm rotors. It also provides high power decoupling and a cross- (CP) set-up, giving operators flexibility to use double CP or traditional CP with no limitation compared to room temperature probes. In addition, the probe includes automatic tuning and matching as well as an automated set-up to adjust the magic angle.

MAS Shuttlefor fully automated solid-state NMR applications

CPMA和HRMAS的MAS班车提供全自动解决方案，以减少动手时间并增加吞吐量。

设备needed:

• iProbe
• Avance Neo Console
• MAS3气动控制单元
• 抽样酶自动化系统

The software, IconNMR, takes full control of running your experiment; from selecting the sample to co-ordinating the insertion, getting the rotor up to spin speed, and returning it safely back to its original position.

一旦你充满了SampleCase, your experiments can run unattended, increasing your instrument efficiency with automated operation. Samples can be run overnight or over weekends.

Solid State Analysis of Medicines Flyer: