Традиционно в аналитическом приборостроении большое внимание уделяется совершенствованию оборудования, повышению чувствительности регистрирующих систем и т.д. Сегодня в аналитической хроматографии разделение даже самых сложных смесей совершается рутинно с использованием стандартных приемов, и при этом время анализа обычно не превышает нескольких минут. Однако, сложилась такая ситуация, что пробоподготовка образца занимает в несколько раз больше времени, чем его анализ.

Альтернативой традиционному методу пробоподготовки в жидкостной хроматографии — жидкостной экстракции — может быть экстракция с помощью сверхкритических флюидов. Мы предлагаем жидкостный хроматограф Nexera UC, который включает в себя специализированные модули: LC-30ADSF / SFC-30A для подачи СО2 в качестве подвижной фазы и SFE-30A для сверхкритической флюидной экстракции.

СФХ-МС/МС систему Nexera UC можно использовать для решения самого широкого круга задач, включая разделение и определение изомеров и хиральных молекул в образцах природного происхождения и пищевых продуктах, поиск и идентификацию различных биомаркеров в биологических жидкостях, а также анализ искусственных полимеров.

	Традиционная ВЭЖХ-МС и ГХ-МС:	Nexera UC:
	Сложная, многоступенчатая и времязатратная пробоподготовка	Полностью автоматизированная пробоподготовка, совмещенная с последующим анализом
	Деградация лабильных соединений в процессе пробоподготовки	Даже крайне лабильные соединения могут быть точно определены
	Риск потери следовых количеств целевых соединений в ходе пробоподготовки	Надежное определение следовых количеств целевых соединений в образцах с самой сложной матрицей

Не просто еще одна техника хроматографического разделения, а единый универсальный метод, удовлетворяющий большинство потребностей пользователя

СФХ-МС/МС система Nexera UC кардинальным образом увеличивает эффективность работы аналитической лаборатории, предлагая совершенно новую технологию — Комплексную хроматографию (Unified Chromatography — UC), объединяющую в едином процессе предварительную подготовку образца к анализу, высокоэффективное хроматографическое разделение и высокочувствительное масс-спектрометрическое детектирование.

Примеры практического использования Nexera UC

Разделение изомеров	Хиральный анализ	Выявление и идентификация биомаркеров в крови (анализ методом «сухой капли»)	Быстрая валидация очистки технологического оборудования в фармацевтической промышленности	Анализ синтечиских полимеров: определение добавок/допантов

Определение остаточного содержания пестицидов традиционным методом с использованием пробоподготовки методом QuEChERS и при помощи СФХ-МС/МС системы Nexera UC
Стандартная пробоподготовка методом QuEChERS как правило занимает порядка 35 минут и требует проведения достаточно большого количества ручных операций. При использовании Nexera UC образец готовится к SFE/SFC анализу всего лишь за пять минут, при этом требуется всего одна ручная операция.

СФХ-МС/МС система Nexera UC позволяет идентифицировать и количественно определять сотни индивидуальных соединений различной природы в ходе одного анализа. Например, в случае определения остаточного содержания пестицидов в объектах окружающей среды и/или пищевых продуктах одна Nexera UC может с успехом заменить традиционные методы анализа с помощью ГХ-МС/МС и ВЭЖХ-МС/МС.

► Nexera UC листовка

► Статья «Швейцарский нож химика-аналитика: система для комплексной хроматографии Shimadzu Nexera UC SFE–SFC–MS», журнал «Аналитика», 1/2016 г

Fully automated on-line sample preparation and analysis

Nexera UC on-line SFE-SFC is a revolutionary system that combines on-line SFE and SFC in a single flow path. Target compounds are extracted from solid samples and then automatically transferred to SFC/MS so that no human intervention is required. The Nexera UC on-line SFE-SFC system reduces the time for pretreatment of samples and acquires highly accurate data.

Prevent degradation of labile compounds
With conventional solvent extraction, labile compounds may react with extraction solvents or could be oxidized and/or degraded.

Analysis of biomarkers from dried blood spots (DBS)
Nexera UC can extract a trace amount of liquid samples. For biomarker validation, the preparation requires simply enclosing a blood spot in the 0.2 mL special extraction vessel.

Only a few simple preparation steps for cleaning validation
Nexera UC can be applied to cleaning validation which is performed in the pharmaceutical industry to confirm that manufactuaring equipment has been properly cleaned. Nexera UC automatically runs a series of steps from extraction to analysis, by only putting the sample swab in the extraction vessel. In conventional cleaning validation, the sample swab needs to be extracted with water, and then the extraction is analyzed by TOC. However, when a target compound is hydrophobic, swab extraction is performed with ethanol and TOC is not applicable. Nexera UC is capable of performing both types of cleaning validation.

Supercritical fluid extraction of trace additives in polymers
Polymer additives are widely used to prevent optical or thermal degradation, or to enhance functionalities. An example, Irganox 1010, is insoluble in THF or Chloroform, and hard to sublime. Therefore, analysis by GPC or GC is difficult. By simply homogenizing a sample and enclosing it in the extraction vessel, Nexera UC can detect labile or trace quantities of additives.

For Research Use Only. Not for use in diagnostic procedures.

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Unified speed of analysis, sensitivity, and resolution

Solutions provided by Nexera UC

• Very fast separation speed due to the relatively low viscosity of supercritical fluid
• Improved peak capacity and chromatographic resolution
• Efficient separation of analogues and/or chiral compounds by high penetration mobile phase
• Different separation mode leads to high sensitivity
• Improved sensitivity resulting from split-less introduction into detector
• Reduction of environmental impacts and costs by reducing amount of organic solvents needed

Higher resolution
Improved separation and detection capabilities result from the low viscosity and high diffusion coefficient of supercritical fluid. As shown below, Nexera UC demonstrates high-separation selectivity for isomeric compounds that are difficult to separate by conventional LC.

Sensitivity results from different separation modes in HPLC vs SFC
Using SFC in front of a mass spectrometer offers greater sensitivity than achieved with LC/MS/MS.

Enhanced sensitivity using splitless transfer to MS
Low dead volume back pressure regulator suppresses diffusion of peaks and can transfer the total eluate directly to an mass spectrometer to achieve higher sensitivity.

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Easy and efficient method scouting for separating chiral compounds

Automatically performs a variety of method scouting processes
The high-speed performance of SFC can shorten the time required for method scouting. It automatically generates a large number of methods by utilizing combinations of up to 12 columns, four modifiers, and a different ratios of modifiers to mobile phase.

Chiral analysis with «Nexera UC Chiral Screening System»
CHIRALPAK® Series and CHIRALCEL® Series columns (Daicel Corporation) for chiral analysis are capable of resolving a wide variety of compounds by showing complementary separation targets. The combination of the Nexera UC Chiral Screening System and these columns simplifies method scouting for chiral analysis.

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Customized modules for Nexera UC based on Nexera technology
Supercritical Fluid Extraction Unit SFE-30A
This unit operates at a maximum temperature of 80°C to allow faster and more complete extractions. Two sizes of extraction vessels (5 mL and 0.2 mL) can be chosen based on the sample amount. This unit has the internal capacity to run up to four samples automatically; with the addition of an optional rack changer, it can accommodate unattended operation for up to 48 samples.

CO2 Delivery Unit LC-30ADSF/Backpressure Control Unit SFC-30A
Stable baseline with low pulsation is realized by LC-30 ADSF with a built-in cooler for pump heads, which delivers mobile phases up to 5 mL/min at pressures up to 66 MPa. The low dead volume of SFC-30A (0.7 uL) allows a mass spectrometer to be directly connected to the SFC system with out splitting so that higher sensitivity can be achieved.

Nexera UC reduces environmental impact
Comparison of costs and consumption of organic solvent for a single analysis by conventional normal-phase LC vs. SFC is shown below. By using SFC, the total cost of analysis is reduced by 87.6% and the consumption of organic solvent is reduced by 94.2%.

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For Research Use Only. Not for use in diagnostic procedures.

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Nexera UC Awards

2015 R&D magazine Award
The award from R&D magazine recognizes Shimadzu’s Nexera UC system as one of the 100 most technically significant new products of the year in the analytical and testing category. R&D Magazine chose the Nexera UC system because its fully automated technology opens up new analytical opportunities in many fields, including food products, drug discovery and delivery, chemicals, pharmaceuticals, and cleaning validation. With industry-leading throughput and superior levels of sensitivity, the system eliminates the need for complicated sample pre-treatment and reduces the possibility of human error during analysis.

Pittcon Editors’ Gold Award 2015
The Pittcon Editors’ Awards recognize the most innovative products presented at Pittcon for the first time based on votes by the media corps. Editors awarded the Nexera UC for its ability to provide a workflow solution that addresses the bottleneck in real-world sample analyses.

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SFC/UHPLC Switching System

The Nexera UC LC/SFC switching system makes it easy to switch between LC and SFC just by adding a single LC pump to an SFC system. By utilizing this system, conventional LC analysis can be performed as usual. At the same time, with samples that are difficult to separate using LC, conditions can be investigated with SFC which has different separation modes than LC.

Enables Both UHPLC and SFC Analysis Using a Single System
Various methods are needed to separate chiral compounds, structural isomers, and other such substances in all sorts of fields, such as pharmaceuticals, foods, and environmental testing. Because supercritical fluid chromatography (SFC), which uses supercritical CO2 as a mobile phase, exhibits different separation behavior than ultra high performance liquid chromatography (UHPLC), superior separation results can be quickly obtained during method development by screening with both SFC and UHPLC separation methods.

Reduced Laboratory Space Requirements and Equipment Costs
By simply adding one solvent delivery unit to a standard SFC system, both SFC analysis and UHPLC analysis can be performed using a single system. Sharing the solvent delivery unit (for pumping organic solvents), autosampler, column oven, and detector for both SFC and UHPLC analysis minimizes space requirements and equipment cost and improves the equipment utilization rate. Moreover, this allows for selection of the optimal column from among a combined total of up to 12 SFC and UHPLC columns, when performing method scouting.

Software Performs the Work of Switching Between SFC and UHPLC
Purging of mobile phases, which is required when switching between SFC and UHPLC, is accomplished by simply executing a batch table automatically generated by the dedicated software. That means even first-time users can smoothly switch between SFC and UHPLC analysis. It also enables multiple mobile phases and columns to be used for method scouting. No reconnecting of flow lines is required when switching from SFC to UHPLC (or from UHPLC to SFC). Consequently, the system can switch continuously between both analysis modes without being affected by the preceding mode.

Reliable Analysis Even When Switching Between SFC and UHPLC Modes
SFC and UHPLC involves significantly different mobile phases and separation characteristics, but analysis can be performed reliably without effects from switching modes by simply purging the flow lines.

Using the System for Chiral Analysis
In this example, methods were scouted for two types of chiral standard samples using both SFC and UHPLC. UHPLC and SFC parameter settings in the method scouting software can be specified by clicking a button to switch between modes.

A comparison of SFC/UHPLC chromatograms using three different columns indicated that UHPLC parameters provided better separation for omeprazole and SFC parameters provided better separation for imdapamide. LabSolutions software makes it easy to compare chromatograms from multiple sets of data.

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