Shimadzu Corporation

Shimadzu Co.

Przemyslaw Stasica

Bob Boughtflower

Tomoyuki Yamazaki

Yutaka Kono

Masayuki Nishimura

Yosuke Iwata

In a preparative separation-purification system for passing a solution containing a target component through a trap columnto capture the target component in the column, and for subsequently passing an eluting solvent through the columnto elute the captured component and collect it in a container, an outlet apertureof the columnhas a tapered shape whose sectional area is largest on a plane facing an inner space of the columnand decreases in the flowing direction of the liquid. A filterfor preventing deposition of the target component is also provided at the boundary between the inner space of the columnand a passage for discharging liquid from the inner space. By this configuration, clogging of the passage at the outlet end of the columndue to deposition of the target component is prevented.

Preparative separation-purification system

Provided is a gas-blowing vaporizing and drying device, which includes: a sample tube in the form of a double tube including an inner tube for a solution and an outer tube for a gas, the inner tube protruding from one end of the outer tube by length L; and a collection container including a container body and a lid provided with a protrusion sleeve tube, the protrusion sleeve tube including a coupling portion at an end to be located outside the container body and a sleeve portion of a length equal to or longer than L having an open end to be located inside the container body, the coupling portion being designed to be coupled to the aforementioned one end of the outer tube in an air-tight manner.

Gas-blowing vaporizing and drying device

Provided is a gas-blowing vaporizing and drying device for blowing gas at a solution containing a target component, and thus nebulizing the solution to promote vaporization of the solvent while dropping the solution into the collection container, in which contamination does not occur even if different solutes are successively powderized. In the gas-blowing vaporizing and drying device according to the present invention, a capto be fitted to the upper opening of a collection container bodyincludes: a solution-introducing tubeA for introducing a solution supplied from a passage, into a collection container; a gas-introducing tubeB for introducing a gas supplied from a passage, into the collection container; and an exhaust portC. Further, the exhaust portC includes a filterD for preventing the powderized solute from passing therethrough.

Gas blowing vaporizing and drying device

In a preparative separation-purification system for passing a solution containing a target component through a trap column to capture the target component in the column, and for subsequently passing an eluting solvent through the column to elute the captured component and collect it in a container, a dilution passage is merged with a collection passage for sending an eluate from the outlet end of the trap column to the collection container, and a diluting liquid is intermittently introduced through the dilution passage into the collection passage. The diluting liquid lowers the concentration of the target component in the eluate and impedes the deposition of the target component. Thus, clogging of the passage due to the deposition of the target component eluted from the trap column is effectively prevented.

Preparative separation-purification system for capturing target components

A liquid leakage between a needle and a needle port is prevented. To this end, a guide section, a passage section, and a tapered section are provided in an in-port path of a needle port. The guide section has an inside diameter larger than the outside diameter of a body of a needle. The passage section has an inside diameter smaller than the outside diameter of the body of the needle and larger than the tip diameter of a tapered portion of the needle. The tapered section connects the guide section and the passage section. The taper angle &#x3b8;of the tapered section is set to be larger than the taper angle &#x3b8;of the tapered portion of the needle, and the width w of the tapered section is set to be smaller than half the difference between the outside diameter of the body and the tip diameter of the needle.

Needle port

Collection containers () are heated by head conduction from a container rack () with a heater () as the heat source. When an eluting solvent is supplied into a trap column () by a pump (), an eluate containing a target compound exiting from the column () flows through a preparative separation passage () and drips from a solution nozzle (), and this solution is separated into fine droplets by a gas stream blowing from a gas ejection nozzle (). When a droplet touches an inner wall of the container (), the volatile solvent immediately vaporizes, leaving the target compound precipitated in solid forms on the inner wall. Thus, the process of vaporizing and drying the eluate to collect the target compound is completed within a short period of time. This process can be performed online and hence is suitable for laborsaving.

Preparative separation/purification system

A needle washing mechanism allowing the selection of an appropriate needle cleaning liquid without having to take volatility into consideration is presented. The needle washing mechanism has: needles standing on a base side by side and each of which has a path inside thereof through which a liquid passes; washing ports having washing holes including openings; and a needle cleaning liquid supply means for supplying a needle cleaning liquid to each of the washing holes, and includes cap sections, which are provided on the outer circumferential surface of the needles, for closing the openings of the washing holes when the needles are inserted into the washing holes. The washing ports are biased toward the openings by means of biasing means. In addition, disposal passages for discharging the needle cleaning liquid from the washing holes are provided in the washing ports.

Needle washing mechanism

A solution containing a target compound is passed through a trap column () to capture the target compound in the column (). Thereafter, wash water is introduced in the trap column (). Then, the setting of a six-port valve () is changed and an on/off valve () is opened to introduce nitrogen gas through a supply-side passage () in the trap column (). In this stage, the nitrogen gas is warmed by means of a heat-exchange block (), and the trap column () is warmed via a column rack (). Any water remaining in the trap column () is initially thrust upwards by the nitrogen gas, to be extruded from an exit edge () and discharged through a discharge-side passage (). Furthermore, any water adhering to adsorbent or the inner wall surface of the trap column () is quickly vaporized and carried away by the nitrogen gas. In this manner, any water remaining in the trap column () can be rapidly removed, so that no water will be included in an eluate in the subsequent stage where a solvent with a strong elution power is introduced into the trap column () to collect the eluate. Thus, the eluate is rapidly vaporized and dried, so that the target compound in solid forms can be efficiently collected.

A fractionating and refining device includes a solution sending flow path for supplying a solution, including a fractionated target component, a gas supply flow path, a collecting vessel, a warming mechanism for warming the collecting vessel, and a probe formed by integrating tip end portions of the solution sending flow path and the gas supply flow path with each other. A lid of the vessel includes a solution inlet to which the tip end portion of the solution sending flow path is connected, gas inlets to which the tip end portion of the gas supply flow path is connected, and gas discharge ports connecting an inside and an outside of a vessel main body of the vessel.

Fractionating and refining device

A mixed liquid passage () is connected to a trapping passage () at a point upstream of a trap column (). A mixture of a diluting liquid and an additive agent, which are respectively drawn and sent by pumps () and (), is supplied into the mixed liquid passage (). When an eluate containing a target compound is passed through the trap column (), the eluate is diluted with the diluting liquid and hence its elution capability decreases, so that the target compound can be easily captured in the trap column (). Meanwhile, the solubility of the mobile phase in the eluate decreases, causing not only the target component but also foreign compounds to more easily precipitate. However, their precipitation is prevented by the effect of the additive agent. Thus, clogging of the trap column () or pipes is prevented.

The present invention aims at providing a preparative separation/purification system for vaporizing an eluate in a short period of time, while enhancing the efficiency of collecting the target substance by accelerating the initiation of collecting the eluate. The preparative separation/purification system in which water containing a target component is passed through a columnto capture the target component in the columnand then a solvent is passed through it to collect the target compound, includes: a liquid supply meansfor supplying a solvent to the column, with the target component captured in the column, while the columnis vertically held with the inlet end thereof directed downwards and the discharge end thereof directed upwards, the solvent having a low solubility to water and having a specific gravity greater than that of water; a passage selection meansfor changing the passage configuration so that a solution exiting from the columnis selectively sent to either a collection passageor a disposal passage; a passage control meansfor controlling the passage selection meansso that, when water exits from the column, the water is sent to the disposal passage, and when solution containing solvent exits from the column, the solution is sent to the collection passage; and a flow rate control meansfor controlling so that the water is supplied at a first flow rate to the disposal passage, and the solution containing solvent is supplied to the collection passageat a flow rate lower than the first flow rate.

After a target compound is captured by an adsorbent within a trap column () held by a column rack () in a substantially vertical position and the column is filled with water to wash its inside, dichloromethane is slowly introduced from an inlet end () on the lower side by a pump (). The water within the trap column () is pushed upward by dichloromethane and exits from an outlet end (), to be disposed of via a two-way selector valve () and a disposal passage (). Dichloromethane elutes the captured target compound. Therefore, when the eluate, which initially consists of water, changes via an emulsion to dichloromethane, the eluate contains an adequately high concentration of target compound. At this point, the two-way valve () is switched to a preparative separation passage (). As a result, a solution that is adequately free from water and yet contains the target compound can be collected into a collection container (), and the target compound in solid forms can be quickly obtained.

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Hertfordshire, United Kingdom

Przemyslaw Stasica