CN209327285U - A kind of circulatory system of high performance liquid chromatograph mobile phase - Google Patents

A kind of circulatory system of high performance liquid chromatograph mobile phase Download PDF

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Publication number
CN209327285U
CN209327285U CN201821493060.1U CN201821493060U CN209327285U CN 209327285 U CN209327285 U CN 209327285U CN 201821493060 U CN201821493060 U CN 201821493060U CN 209327285 U CN209327285 U CN 209327285U
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mobile phase
high performance
performance liquid
solenoid valve
liquid chromatograph
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范军
黄小锋
张晨梁
闻晓光
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TAIZHOU OVERSEAS PHARMACEUTICAL Ltd.
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Taizhou Cheng Yi Pharmaceutical Development Co Ltd
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Abstract

The utility model discloses a kind of circulatory systems of high performance liquid chromatograph mobile phase, it includes high performance liquid chromatograph (1), solenoid valve (2), mobile phase collection device (4) and waste collecting device (5);The entrance of high performance liquid chromatograph (1) mobile phase outlet connection solenoid valve (2), the solenoid valve includes at least two outlets, the outlet includes collecting loop exit and waste liquid port, the entrance for collecting loop exit connection mobile phase collection device (4);The entrance of waste liquid port connection waste collecting device (5);The high performance liquid chromatograph (1) is adapted with solenoid valve (2).The utility model can fast implement recycling for mobile phase of high performance liquid chromatography, have the advantages that online recycling circulation, flexible operation, safety and stability and cost is relatively low.

Description

A kind of circulatory system of high performance liquid chromatograph mobile phase
Technical field
The utility model patent is related to chromatograph analysis technical field, specially a kind of high performance liquid chromatograph mobile phase The circulatory system.
Background technique
High performance liquid chromatography is almost to spread each neck of quantitative and qualitative analysis at present using most chromatogram analysis methods Domain.Highly effective liquid phase chromatographic system is made of mobile phase liquid storage bottle, infusion pump, sample injector, chromatographic column, detector and logger.Make With high-efficient liquid phase color time spectrum, liquid object to be detected is mutual due to different material in measured object and stationary phase by injection chromatographic column Effect is different, is moved by being eluted in stationary phase for mobile phase, and the sequence that different material leaves chromatographic column is different, passes through detection Device can obtain different peak-to-peak signals, judge the substance contained by determinand finally by these signals are analysed and compared.It is using When high performance liquid chromatography is analyzed, the dosage of mobile phase is very big, and especially plant-scale efficient liquid phase separation needs to expend A large amount of expensive chromatographic grade solvents.The waste liquid generated at present for high-efficient liquid phase analysis is all to carry out special waste liquid after collecting Processing, whole process is complicated and time-consuming, and higher cost.
The technology in terms of high performance liquid chromatograph mobile phase recycles includes following several at present:
CN201965119U utility model patent discloses a kind of mobile phase of high performance liquid chromatography recycling device, A waste tank is connect behind high performance liquid chromatograph, then connects a rectifying column, waste liquid collects fraction after rectifying is cooling, then It recycles.The device, which need to reach industrial production scale, just can be used, and cost is very high, needs to install a large amount of rectifying and sets Standby, flexibility is poor, needs to add up that certain waste liquid is just rectifiable recycles primary, and technical difficulty is high.
CN201514402U utility model discloses a kind of high-performance chromatograph for circulating liquid phase, by liquid storage device, mixer, high pressure Pump, sample injector, chromatographic column, detector and recorder composition, are equipped with level-one flow channel switching valve, level-one between mixer and high-pressure pump Flow channel switching valve output end is connected with liquid-drop machine, and liquid-drop machine passes through the output port of second level flow channel switching valve connecting detection device, drop Liquid device is made of funnel and dropper, and funnel bottom connects level-one flow channel switching valve, and dropper connects second level flow channel switching valve, this is practical It is novel that mobile phase and sample is only allowed to carry out separating for several times by chromatographic column over and over again, to reach the more difficult separate substance of separation Purpose, mobile phase can not be recycled.
CN205139101U utility model discloses a kind of chromatogram flow phase recycling device, which is divided to two kinds of function Can, for gas-chromatography, connect first compressor behind chromatograph, output is terminated with fractionating column, then connect the second compressor, Ice chest, gasifier, recycling enter gas chromatograph and recycle;For high performance liquid chromatography, then device and patent CN201965119U is similar.The preparation method takes a long time, and technical difficulty is higher, needs further distilation, it is difficult to realize Quickly recycling, it is also desirable to which reaching industrially scalable just can be used, and not be suitable for researching and developing laboratory.
Utility model content
The purpose of the utility model is to overcome problem of the prior art, provide a kind of following for high performance liquid chromatograph mobile phase Loop system.
A kind of circulatory system of the high performance liquid chromatograph mobile phase of the utility model, it include high performance liquid chromatograph, Solenoid valve, mobile phase collection device and waste collecting device;The high performance liquid chromatograph mobile phase outlet connection solenoid valve Entrance, the solenoid valve include at least two outlets, and the outlet includes collecting loop exit and waste liquid port, the collection circulation The entrance of outlet connection mobile phase collection device;The entrance of the waste liquid port connection waste collecting device;The high-efficient liquid phase color Spectrometer is adapted with solenoid valve.
It as a further improvement of the utility model, further include guard column, the guard column is set to solenoid valve and mobile phase Between collection device, the outlet connection mobile phase of the entrance for collecting loop exit connection guard column, the guard column is collected The entrance of device.
The high performance liquid chromatograph includes detector as a further improvement of the utility model, the detector with Solenoid valve is connected by control circuit and is adapted to, and the control circuit is equipped with photosignal control switch, the photosignal control The peak-to-peak signal that system switch is detected with detector is adapted.
The solenoid valve is connected with timing control switch as a further improvement of the utility model,.
The solenoid valve includes direct-acting electromagnetic valve, backpulsing solenoid valve as a further improvement of the utility model, Or guide electromagnetic valve.
The utility model also provides a kind of high performance liquid chromatograph mobile phase as a further improvement of the utility model, The control method of the circulatory system, the following steps are included:
Step S110: preparing the mobile phase of efficient liquid phase detection, carries out the isocratic detection of efficient liquid phase;
Step S120: judging whether the access of solenoid valve waste liquid port is opened, if then carrying out step S130, if otherwise carrying out Step S140:
Mobile phase: being passed through in waste collecting device by step S130 by the waste liquid port of solenoid valve, at subsequent progress waste liquid Reason, returns to step S120;
Step S140: mobile phase is passed through in mobile phase collection device by the collection loop exit of solenoid valve, is being passed through Before mobile phase collection device, it may be selected to filter by guard column, be then passed through in mobile phase collection device again;Then mobile phase can It is passed directly into high performance liquid chromatograph inlet, can also be retained in mobile phase collection device and be used to next time, to complete Circulation repeatedly utilizes, and returns to step S120.
Whether the access of the solenoid valve waste liquid port in the step S120 is opened, and needs according in high performance liquid chromatograph Detector testing result judges, passes through photosignal by the detector of high performance liquid chromatograph 1 according to the result of judgement and controls Solenoid valve opens the channel selector of different outlets.
The foundation of the judgement as a further improvement of the utility model, are as follows: when detector detects sample optical telecommunications Number when, then may determine that at this time mobile phase include impurity, then open the access of waste liquid port;When sample photoelectricity is not detected in detector When signal, then it may determine that mobile phase does not include impurity at this time, then the access of waste liquid port is not opened, and is opened and is collected loop exit Access.
Whether the access of the solenoid valve waste liquid port in the step S120 is opened as a further improvement of the utility model, It is set by timing control switch, according to the access and waste liquid of the collection loop exit of the appearance time setting solenoid valve of detection substance Mouthful time for opening respectively of access, when the appearance time for reaching detection substance, then the access for controlling waste liquid port is opened, remaining when Between for collect loop exit access open period.
The opening time of the access of the waste liquid port is not less than appearance time as a further improvement of the utility model, Duration.
The control circuit is photosignal control access as a further improvement of the utility model,;The timing control System switch is that time control solenoid valve switchs.
The utility model compared with prior art, has the following advantages that.
The circulatory system of the high performance liquid chromatograph mobile phase of the utility model include high performance liquid chromatograph, solenoid valve, Guard column, mobile phase collection device and waste collecting device have recycling circulation fast by the mutual cooperation between each component Speed has the advantages that online recycling circulation, flexible operation, safety and stability and cost is relatively low.
Further, the utility model provides the control mode of two kinds of electromagnetic valve switch, and a kind of mode is by efficient The photosignal access control that liquid chromatograph detector issues;Another mode is that set-up time control is opened on solenoid valve It closes, is controlled by the duration of setting opening and closing, can flexibly be used cooperatively demand, select different control methods.
The circulatory system and its control method of the high performance liquid chromatograph mobile phase of the utility model be both able to satisfy industrialization Mass production, use when being also able to satisfy laboratory research and development can be avoided the unnecessary waste of existing experiment research and development, also being capable of root Expand the circulatory system according to ratio and meets the needs of industrialized production.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the circulatory system of the high performance liquid chromatograph mobile phase of the utility model.
Fig. 2 is the structural schematic diagram of embodiment 2.
Fig. 3 is the matching relationship schematic diagram that the access of the collection loop exit of embodiment 8 is opened.
Fig. 4 is the matching relationship schematic diagram that the access of the waste liquid port of embodiment 8 is opened.
The high-efficient liquid phase chromatogram spectrum that Fig. 5 is compound A in embodiment 9.
Fig. 6 is the matching relationship schematic diagram that the access of the collection loop exit of embodiment 9 is opened.
Fig. 7 is the matching relationship schematic diagram that the access of the waste liquid port of embodiment 9 is opened.
In figure: 1- high performance liquid chromatograph, 2- solenoid valve, 3- guard column, 4- mobile phase collection device, 5- waste collection dress It sets, 6- control circuit, 7- timing control switch.
Specific embodiment
Explanation that the utility model is further explained with reference to the accompanying drawings and examples.
Embodiment 1
A kind of circulatory system of high performance liquid chromatograph mobile phase, it includes high performance liquid chromatograph 1, solenoid valve 2, flowing Phase collection device 4 and waste collecting device 5;The entrance of 1 mobile phase of the high performance liquid chromatograph outlet connection solenoid valve 2, institute Stating solenoid valve includes at least two outlets, and the outlet includes collecting loop exit and waste liquid port, and the collection loop exit connects Connect the entrance of mobile phase collection device 4;The entrance of the waste liquid port connection waste collecting device 5;The high performance liquid chromatograph 1 It is adapted with solenoid valve 2.
Embodiment 2
The circulatory system of the utility model high performance liquid chromatograph mobile phase further includes guard column 3, and the guard column 3 is set Between solenoid valve 2 and mobile phase collection device 4, the entrance for collecting loop exit connection guard column 3, the guard column 3 Outlet connection mobile phase collection device 4 entrance.Remaining is consistent with the scheme of embodiment 1.
Embodiment 3
The high performance liquid chromatograph 1 of the circulatory system of the utility model high performance liquid chromatograph mobile phase includes detector, Detector connect adaptation by control circuit 6 with solenoid valve 2, and control circuit is equipped with photosignal control switch, photosignal Control switch is adapted with the peak-to-peak signal that detector detects.Remaining is consistent with the scheme of embodiment 1 or 2.
Embodiment 4
The solenoid valve 2 of the circulatory system of the utility model high performance liquid chromatograph mobile phase is connected with timing control switch 7. Remaining is consistent with embodiment 1-3 either a program.
Embodiment 5
The solenoid valve 2 of the circulatory system of the utility model high performance liquid chromatograph mobile phase includes direct-acting electromagnetic valve, anti- Rush formula solenoid valve or guide electromagnetic valve.Remaining is consistent with embodiment 1-4 either a program.
Embodiment 6
The utility model also provides a kind of control method of the circulatory system of high performance liquid chromatograph mobile phase, including following Step:
Step S110: preparing the mobile phase of efficient liquid phase detection, carries out the isocratic detection of efficient liquid phase;
Step S120: judging whether the access of 2 waste liquid port of solenoid valve is opened, if then carrying out step S130, if otherwise into Row step S140:
Mobile phase: being passed through in waste collecting device 5 by step S130 by the waste liquid port of solenoid valve, at subsequent progress waste liquid Reason, returns to step S120;
Step S140: mobile phase is passed through in mobile phase collection device by the collection loop exit of solenoid valve, is being passed through Before mobile phase collection device 4, it may be selected to filter by guard column 3, be then passed through in mobile phase collection device 4 again;Then flow It mutually can be passed directly into 1 inlet of high performance liquid chromatograph, can also be retained in mobile phase collection device 4 and be used to next time, from And complete circulation and repeatedly utilize, return to step S120.
Embodiment 7
The control method of the circulatory system of the utility model high performance liquid chromatograph mobile phase, the electromagnetism in step S120 Whether the access of 2 waste liquid port of valve is opened, and needs to be judged according to the detector testing result in high performance liquid chromatograph 1, according to The result of judgement controls the access that solenoid valve 2 opens different outlets by photosignal by the detector of high performance liquid chromatograph 1 Switch;Remaining is consistent with the scheme of embodiment 6.
Embodiment 8
The control method of the circulatory system of the utility model high performance liquid chromatograph mobile phase, the foundation of judgement are as follows: when When detector detects sample photosignal, then it may determine that mobile phase includes impurity at this time, then opens the access of waste liquid port;When When sample photosignal is not detected in detector, then it may determine that mobile phase does not include impurity at this time, then the access of waste liquid port is not It opens, opens the access for collecting loop exit.Remaining is consistent with the scheme of embodiment 7.
As shown in figure 3, when carrying out the isocratic detection of efficient liquid phase, when the detector in high performance liquid chromatograph 1 is not detected When sample photosignal, the access that solenoid valve 2 opens connection guard column 3, mobile phase free from foreign meter are controlled by control circuit 6 By the filtering of guard column 3, it is collected into mobile phase mobile phase collection device 4, high performance liquid chromatograph 1 is again introduced into and recycles benefit With.
As shown in figure 4, when carrying out the isocratic detection of efficient liquid phase, when the detector in high performance liquid chromatograph 1 detects sample When product photosignal, the access that solenoid valve 2 opens connection waste collecting device 5, the stream containing impurity are controlled by control circuit 6 Dynamic phase is discharged to waste collecting device 5.
Above-mentioned solenoid valve 2 includes direct-acting electromagnetic valve, backpulsing solenoid valve or guide electromagnetic valve.
Embodiment 9
The control method of the circulatory system of the utility model high performance liquid chromatograph mobile phase, the electromagnetism in step S120 Whether the access of 2 waste liquid port of valve is opened is set by timing control switch, according to the appearance time setting solenoid valve 2 of detection substance The time that the access of the access and waste liquid port of collecting loop exit is opened respectively is then controlled when the appearance time for reaching detection substance The access of waste liquid port processed is opened, remaining time is the period collecting the access of loop exit and opening.The side of remaining and embodiment 6 Case is consistent.
As shown in Figure 5,6, when carrying out the isocratic detection of efficient liquid phase, according to the appearance time 1.3-1.8min of compound A, The time of the access of setting opening connection guard column 3 is 02:00-04:00 on 2 clock switch of solenoid valve, has arrived the time of setting Point is i.e. from 2 minutes to 4 minute, and the switch of solenoid valve 2 is opened, and mobile phase free from foreign meter passes through the filtering of guard column 3, is collected into stream Dynamic phase mobile phase collection device 4, is again introduced into high performance liquid chromatograph 1 and recycles.Except the period of setting, solenoid valve The access of 2 connection guard columns 3 is in close state, and when detecting next sample, has arrived the period of setting, switch is beaten again It opens.
As shown in attached drawing 5,7, when carrying out the isocratic detection of efficient liquid phase, according to the appearance time 1.3-1.8min of compound A, The time that the access of connection waste collecting device 5 is opened in setting on 2 clock switch of solenoid valve is 00:00-02:00, to setting The time point set, the switch of solenoid valve 2 was opened, and the mobile phase containing impurity is discharged to waste collecting device 5 i.e. from 0 minute to 2 minute. Except the period of setting, the access that solenoid valve 2 connects waste collecting device 5 is in close state, when the next sample of detection When, the period of setting is arrived, switch is again turned on.
Above-mentioned solenoid valve 2 includes direct-acting electromagnetic valve, backpulsing solenoid valve or guide electromagnetic valve.
Embodiment 10
The control method of the circulatory system of the utility model high performance liquid chromatograph mobile phase, the access of waste liquid port are beaten ETAD expected time of arrival and departure is not less than the duration of appearance time.Remaining is consistent with the scheme of embodiment 9.
Above content is the example and explanation of the utility model, but does not mean that the obtainable advantage of the utility model by this Limitation may be realized in the simple transformation, and/or some embodiments to structure in all the utility model practice processes excellent Wherein one or more of point are within the scope of protection of this application.

Claims (5)

1. a kind of circulatory system of high performance liquid chromatograph mobile phase, it is characterised in that: it include high performance liquid chromatograph (1), Solenoid valve (2), mobile phase collection device (4) and waste collecting device (5);High performance liquid chromatograph (1) the mobile phase outlet The entrance of solenoid valve (2) is connected, the solenoid valve includes at least two outlets, and the outlet includes collecting loop exit and waste liquid Mouthful, the entrance for collecting loop exit connection mobile phase collection device (4);The waste liquid port connects waste collecting device (5) Entrance;The high performance liquid chromatograph (1) is adapted with solenoid valve (2).
2. the circulatory system of high performance liquid chromatograph mobile phase according to claim 1, it is characterised in that: it further include protection Column (3), the guard column (3) are set between solenoid valve (2) and mobile phase collection device (4), the collection loop exit connection The entrance of guard column (3), the entrance of outlet connection mobile phase collection device (4) of the guard column (3).
3. the circulatory system of high performance liquid chromatograph mobile phase according to claim 1, it is characterised in that: the efficient liquid Chromatography (1) includes detector, and the detector connect adaptation, the control electricity by control circuit (6) with solenoid valve (2) Road is equipped with photosignal control switch, and the photosignal control switch is adapted with the peak-to-peak signal that detector detects.
4. the circulatory system of high performance liquid chromatograph mobile phase according to claim 1, it is characterised in that: the solenoid valve (2) timing control switch (7) are connected with.
5. the circulatory system of high performance liquid chromatograph mobile phase according to claim 1, it is characterised in that: the electromagnetism Valve (2) includes direct-acting electromagnetic valve, backpulsing solenoid valve or guide electromagnetic valve.
CN201821493060.1U 2018-09-13 2018-09-13 A kind of circulatory system of high performance liquid chromatograph mobile phase Active CN209327285U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109374799A (en) * 2018-09-13 2019-02-22 泰州成医药开发有限公司 A kind of circulatory system and its control method of high performance liquid chromatograph mobile phase

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109374799A (en) * 2018-09-13 2019-02-22 泰州成医药开发有限公司 A kind of circulatory system and its control method of high performance liquid chromatograph mobile phase

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Address after: 225300 room 7806, building D, phase II, new drug creation base, No. 1, Yaocheng Avenue, Taizhou City, Jiangsu Province (east of Chuangye road and north of Yuannan Road)

Patentee after: TAIZHOU OVERSEAS PHARMACEUTICAL Ltd.

Address before: Room 1311, twin tower, No. 1, Yaocheng Avenue, China Pharmaceutical City, Taizhou, Jiangsu 225300

Patentee before: TAIZHOU CHENGYI MEDICINE DEVELOPMENT Co.,Ltd.