JP2008014788A - Liquid chromatograph mass spectrometer - Google Patents

Liquid chromatograph mass spectrometer Download PDF

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JP2008014788A
JP2008014788A JP2006186050A JP2006186050A JP2008014788A JP 2008014788 A JP2008014788 A JP 2008014788A JP 2006186050 A JP2006186050 A JP 2006186050A JP 2006186050 A JP2006186050 A JP 2006186050A JP 2008014788 A JP2008014788 A JP 2008014788A
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pressure
gas
standard sample
liquid
valve
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JP4577280B2 (en
JP2008014788A5 (en
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Tomohito Nakano
智仁 中野
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Shimadzu Corp
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Shimadzu Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To provide an LC/MC equipped with a standard sample introduction part composable with the smaller number of components, while having a function similar to a conventional gas pressure system. <P>SOLUTION: In the standard sample introduction part of the gas pressure system, a pressurized gas passage has a constitution branched from a supply passage of nebulizer gas/drying gas on the downstream side of a flow control valve 21, and linked to a pressurized pipe 51 of a standard sample container 5 through a two-way solenoid valve 6. When sending the standard sample 53, the flow control valve 21 is set at a prescribed value for liquid sending and the two-way solenoid valve 6 is opened, and pressurized gas is introduced into the standard sample container 5 and the two-way solenoid valve 6 is closed instantly, and thereafter the standard sample 53 is sent by accumulated pressure, and simultaneously the nebulizer gas/drying gas is supplied to an ionization part at a prescribed pressure. When stopping liquid sending, the flow control valve 21 is closed and the two-way solenoid valve 6 is opened, to thereby remove a residual pressure. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

本発明は、大気圧イオン化インターフェイスを備えた液体クロマトグラフ質量分析装置に関し、特に、チューニングのために標準試料を導入する標準試料導入部の構成に関する。   The present invention relates to a liquid chromatograph mass spectrometer equipped with an atmospheric pressure ionization interface, and more particularly to a configuration of a standard sample introduction unit that introduces a standard sample for tuning.

液体クロマトグラフ質量分析装置（以下、ＬＣ／ＭＳと略記する）では、質量分析部のチューニングのために所定流量の標準試料を導入する必要がある。チューニングとは、質量分析部の分解能調整、感度調整、質量数校正、イオン化プローブの最適温度設定などを行うことである。   In a liquid chromatograph mass spectrometer (hereinafter abbreviated as LC / MS), it is necessary to introduce a standard sample having a predetermined flow rate for tuning the mass spectrometer. Tuning refers to performing resolution adjustment, sensitivity adjustment, mass number calibration, optimum temperature setting of the ionization probe, and the like.

従来、標準試料を導入する方式として、シリンジポンプ方式とガス圧方式とがある。
シリンジポンプ方式は、例えば特許文献１において提案されているように、シリンジポンプと３方、４方または６方バルブを組み合わせて、シリンジポンプで所定流量の標準試料を加圧して送液するものである。
一方、ガス圧方式は、標準試料容器に収めた標準試料の液面より上の容器内空間に連通する加圧管を通して加圧ガスを導入することにより容器内の液面下に連通する送液管から標準試料を送り出すものである。 Conventionally, as a method for introducing a standard sample, there are a syringe pump method and a gas pressure method.
For example, as proposed in Patent Document 1, the syringe pump system is a combination of a syringe pump and a three-way, four-way, or six-way valve, and pressurizes a standard sample at a predetermined flow rate with a syringe pump to send liquid. is there.
On the other hand, the gas pressure method is a liquid supply pipe that communicates below the liquid level in the container by introducing a pressurized gas through a pressurized pipe that communicates with the space in the container above the liquid level of the standard sample contained in the standard sample container. The standard sample is sent out from

図３にガス圧方式による従来の標準試料導入部の構成例を示す。
大気圧イオン化インターフェイスを備えたＬＣ／ＭＳでは、イオン化プローブにおいて試料を噴霧するためのネブライザガス、或いは、噴霧された液滴中の溶剤の揮発を促進させるためのドライイングガスとして窒素ガスを供給する必要がある。
同図において、１はネブライザガス／ドライイングガスの供給源となるボンベ等のガス源、２はこれらのガスの流量を制御するガスコントロール部であって、流量制御弁２１、圧力ゲージ２２、流路抵抗２３等で構成される。３は調圧弁であって、ネブライザガス／ドライイングガスとガス源１を共有する加圧ガスの圧力を所定圧に調整するものである。４は、３つのポートａ、ｂ、ｃを有する３方電磁弁であって、非励磁状態ではポートｂ−ｃ間が連通し、励磁されるとポートａ−ｃ間が連通するように動作する。なお、ポートｂは大気に通じている。５は、標準試料５３を収容する標準試料容器であって、その内部は液面上空間Ａに連通する加圧管５１と液面下に連通する送液管５２とを介してのみ外部と連通している。７は、過剰な圧力から標準試料容器５を保護する安全弁である。 FIG. 3 shows an example of the configuration of a conventional standard sample introduction unit using a gas pressure method.
In LC / MS equipped with an atmospheric pressure ionization interface, nitrogen gas is supplied as a nebulizer gas for spraying a sample in an ionization probe or as a drying gas for promoting the volatilization of a solvent in sprayed droplets. There is a need.
In the figure, reference numeral 1 denotes a gas source such as a cylinder that serves as a nebulizer gas / drying gas supply source, and 2 denotes a gas control unit that controls the flow rate of these gases, including a flow control valve 21, a pressure gauge 22, It is comprised by the road resistance 23 grade | etc.,. 3 is a pressure regulating valve, which adjusts the pressure of the pressurized gas sharing the gas source 1 with the nebulizer gas / drying gas to a predetermined pressure. Reference numeral 4 denotes a three-way solenoid valve having three ports a, b, and c, which operate so that the ports bc communicate with each other in a non-excited state and communicate with each other when excited. . The port b communicates with the atmosphere. Reference numeral 5 denotes a standard sample container that accommodates a standard sample 53, and the inside thereof communicates with the outside only through a pressurizing pipe 51 that communicates with the space A above the liquid level and a liquid feeding pipe 52 that communicates below the liquid level. ing. A safety valve 7 protects the standard sample container 5 from excessive pressure.

このような構成において、標準試料導入は以下のように行われる。
通常分析時はガス源１から供給された窒素ガスが、ネブライザガスまたはドライイングガスとしてガスコントロール部２で例えば圧力３００ｋＰａ程度に調節されてイオン化部へ流れている。流量は、ネブライザガスの場合は１．５Ｌ／ｍｉｎ程度、ドライイングガスの場合は２０Ｌ／ｍｉｎ程度である。一方、同じガス源１から分岐された加圧ガスは非励磁状態にある３方電磁弁４の入口（ポートａ）で止められている。 In such a configuration, standard sample introduction is performed as follows.
During normal analysis, nitrogen gas supplied from the gas source 1 is adjusted to a pressure of, for example, about 300 kPa by the gas control unit 2 as a nebulizer gas or a drying gas and flows to the ionization unit. The flow rate is about 1.5 L / min for nebulizer gas and about 20 L / min for drying gas. On the other hand, the pressurized gas branched from the same gas source 1 is stopped at the inlet (port a) of the three-way solenoid valve 4 in a non-excited state.

標準試料５３を送液するときは、３方電磁弁４に通電する。これによりポートａ−ｃ間が連通し、調圧弁３で１００ｋＰａ程度に調圧された加圧ガスが加圧管５１を経て標準試料容器５内の液面上空間Ａに導入され、これに押されて標準試料５３が送液管５２を通って図示しないイオン化プローブに向けて送液され、そこでイオン化されて図示しない質量分析部に導入される。
送液を止めるには、３方電磁弁４の通電を停止する。これによりポートｂ−ｃ間が連通するので標準試料容器５内の圧力が大気圧となることで送液が止まる。送液流量は調圧弁３の圧力設定により調節され、通常は５０μＬ／ｍｉｎ程度であり、チューニングにはおよそ３０分を要するから、送液量は１回のチューニング当たり約１．５ｍＬとなる。 When the standard sample 53 is fed, the three-way solenoid valve 4 is energized. As a result, the ports a-c communicate with each other, and the pressurized gas regulated to about 100 kPa by the pressure regulating valve 3 is introduced into the space A above the liquid level in the standard sample container 5 through the pressurized pipe 51 and pushed by this. Then, the standard sample 53 is fed through a liquid feeding tube 52 toward an ionization probe (not shown), where it is ionized and introduced into a mass analysis unit (not shown).
In order to stop liquid feeding, the energization of the three-way solenoid valve 4 is stopped. As a result, the ports bc communicate with each other, so that the liquid feeding stops when the pressure in the standard sample container 5 becomes atmospheric pressure. The liquid feeding flow rate is adjusted by the pressure setting of the pressure regulating valve 3 and is usually about 50 μL / min. Since tuning requires about 30 minutes, the liquid feeding amount is about 1.5 mL per tuning.

特開平９−１５９６６１号公報JP-A-9-159661

上記のように、大気圧イオン化インターフェイスを備えたＬＣ／ＭＳでは、ネブライザガス／ドライイングガスの供給のためにガスの供給源が既に備えられているから、ガス圧方式の場合は加圧ガスのガス源を新たに準備する必要がないこともあって、一般にシリンジポンプ方式よりも低コストで標準試料導入部を構成できる利点がある。
本発明は、さらなるコスト低減のために、従来のガス圧方式と同等の機能を有しながら更に少ない部品点数で構成可能な標準試料導入部を備えたＬＣ／ＭＳを提供することを目的とする。 As described above, in the LC / MS having the atmospheric pressure ionization interface, a gas supply source is already provided for supplying the nebulizer gas / drying gas. Since there is no need to newly prepare a gas source, there is generally an advantage that the standard sample introduction unit can be configured at a lower cost than the syringe pump system.
An object of the present invention is to provide an LC / MS provided with a standard sample introduction part that can be configured with a smaller number of parts while having the same function as the conventional gas pressure method, in order to further reduce the cost. .

本発明は、上記課題を解決するために、ガス圧方式の標準試料導入部において、加圧ガス流路を、ネブライザガス／ドライイングガスの供給流路からその流量制御弁の下流側で分岐し、開閉弁を介して標準試料容器の加圧管に通じるように構成する。
このように構成することにより、少ない部品数で従来と変わらない標準試料導入機能を実現することができる。 In order to solve the above-mentioned problems, the present invention branches the pressurized gas flow path from the nebulizer gas / drying gas supply flow path downstream of the flow control valve in the gas pressure type standard sample introduction section. In addition, it is configured to communicate with the pressurizing tube of the standard sample container through the open / close valve.
With this configuration, it is possible to realize a standard sample introduction function that is the same as the conventional one with a small number of parts.

本発明は上記のように構成されているので、従来構成に比べてコスト削減が可能となる。   Since the present invention is configured as described above, the cost can be reduced as compared with the conventional configuration.

本発明が提供するＬＣ／ＭＳ装置は次のような特徴を有する。即ち、第１の特徴は標準試料導入のための加圧ガス流路をネブライザガス／ドライイングガスの供給流路からその流量制御弁の下流側で分岐するように構成した点にあり、第２の特徴はこの加圧ガス流路を開閉弁を介して標準試料容器の加圧管に通じるように構成した点である。
従って、最良の形態の基本的な構成は、上記２点の特徴的構成を具備するＬＣ／ＭＳ装置である。 The LC / MS apparatus provided by the present invention has the following characteristics. That is, the first feature is that the pressurized gas flow path for introducing the standard sample is configured to branch from the nebulizer gas / drying gas supply flow path downstream of the flow rate control valve. This is characterized in that the pressurized gas flow path is configured to communicate with the pressurized tube of the standard sample container via an on-off valve.
Therefore, the basic configuration of the best mode is an LC / MS apparatus having the above two characteristic configurations.

図１に本発明の一実施例を示す。同図において図３と同一物については図３と同符号を付してあるので再度の説明は省く。
本実施例が図３の従来例と相違する点は、加圧ガスの流路が、ネブライザガス／ドライイングガスの供給流路からその流量制御弁２１の下流側で分岐され、２方電磁弁６を介して標準試料容器５の加圧管５１に通じるように構成されている点である。 FIG. 1 shows an embodiment of the present invention. In this figure, the same components as those in FIG. 3 are denoted by the same reference numerals as those in FIG.
This embodiment is different from the conventional example of FIG. 3 in that the flow path of the pressurized gas is branched from the nebulizer gas / drying gas supply flow path downstream of the flow rate control valve 21. 6 through the pressure tube 51 of the standard sample container 5.

このように構成された本実施例において、標準試料導入は以下のように行われる。
通常分析時は、従来と同様に、ガス源１から供給された窒素ガスが、ネブライザガスまたはドライイングガスとしてガスコントロール部２で調節されてイオン化部へ流れており、流量制御弁２１の下流側で分岐された加圧ガスは非励磁状態にある２方電磁弁６の入口で止められている。
標準試料５３を送液するときは、まず流量制御弁２１の設定圧を送液のための所定圧力（例えば１００ｋＰａ程度）に変更し、続いて２方電磁弁６に短時間（例えば１０秒間）だけ通電して開き、すぐに閉じる。この間に調圧された加圧ガスが加圧管５１を経て標準試料容器５内の液面上空間Ａに導入され、その圧力は２方電磁弁６が閉じた後も蓄えられ、この蓄えられた圧力（蓄圧）により継続的に標準試料５３が送液される。 In the present embodiment configured as described above, the standard sample is introduced as follows.
At the time of normal analysis, the nitrogen gas supplied from the gas source 1 is adjusted by the gas control unit 2 as nebulizer gas or drying gas and flows to the ionization unit as in the conventional case, and is downstream of the flow control valve 21. The pressurized gas branched at is stopped at the inlet of the two-way solenoid valve 6 in a non-excited state.
When the standard sample 53 is fed, first, the set pressure of the flow rate control valve 21 is changed to a predetermined pressure for feeding (for example, about 100 kPa), and then the two-way solenoid valve 6 is briefly switched (for example, 10 seconds). Only energize to open and close immediately. During this time, the pressurized gas conditioned is introduced into the space A above the liquid surface in the standard sample container 5 through the pressure tube 51, and the pressure is stored even after the two-way solenoid valve 6 is closed. The standard sample 53 is continuously fed by the pressure (accumulated pressure).

一方、２方電磁弁６が閉じると共に流量制御弁２１の設定をガス供給のための所定圧に戻すことによりネブライザガス／ドライイングガスを正規の流量で供給し、この状態でチューニングを行う。前述したように、チューニングには約３０分を要するが、この間、標準試料容器５内の液面上空間Ａに蓄えられた加圧ガスの圧力低下は、例えば送液流量が５０μＬ／ｍｉｎで液面上空間Ａの容積が３００ｍＬの場合、０．５％程度に過ぎない。
チューニングが終わると、流量制御弁２１を閉止し、次に２方電磁弁６を開く。ネブライザガス／ドライイングガスの流路の末端は大気圧であるから、これにより液面上空間Ａに蓄えられた加圧ガスの残圧が抜け、標準試料５３の送液が止まる。 On the other hand, the two-way solenoid valve 6 is closed and the setting of the flow control valve 21 is returned to a predetermined pressure for gas supply, whereby nebulizer gas / drying gas is supplied at a normal flow rate, and tuning is performed in this state. As described above, tuning requires about 30 minutes. During this time, the pressure drop of the pressurized gas stored in the liquid surface space A in the standard sample container 5 is, for example, a liquid feed flow rate of 50 μL / min. When the volume of the surface space A is 300 mL, it is only about 0.5%.
When tuning is completed, the flow control valve 21 is closed, and then the two-way solenoid valve 6 is opened. Since the end of the nebulizer gas / drying gas flow path is at atmospheric pressure, the residual pressure of the pressurized gas stored in the upper surface space A is thereby released, and the supply of the standard sample 53 is stopped.

図２に本発明の他の実施例を示す。同図において図１と同一物については図１と同符号を付してあるので再度の説明は省く。
本実施例が実施例１と相違する点は、２方電磁弁６と加圧管５１との間の加圧ガスの流路中に調圧弁３を設けたことである。この調圧弁３により、加圧ガスの圧力が一定に保たれるのでチューニング期間中の標準試料５３の送液流量が安定化する。本実施例は、特に送液流量を高精度に保つ必要がある場合に好適であるが、一方、調圧弁３を必要とするので部品点数が増し、コストダウン効果は限定的である。 FIG. 2 shows another embodiment of the present invention. In this figure, the same components as those in FIG. 1 are denoted by the same reference numerals as those in FIG.
The present embodiment is different from the first embodiment in that the pressure regulating valve 3 is provided in the pressurized gas flow path between the two-way electromagnetic valve 6 and the pressurizing pipe 51. Since the pressure of the pressurized gas is kept constant by the pressure adjusting valve 3, the flow rate of the standard sample 53 during the tuning period is stabilized. This embodiment is particularly suitable when the liquid feed flow rate needs to be maintained with high accuracy, but on the other hand, since the pressure regulating valve 3 is required, the number of parts increases and the cost reduction effect is limited.

本実施例における標準試料導入の手順は実施例１の場合とほぼ同様であるが、ただ流量制御弁２１で加圧ガスの圧力を設定する際に、調圧弁３の制御幅を見込んで送液最適圧よりも少し高い圧力に設定すべき点が実施例１の場合と異なる。
また、チューニング終了後、蓄えられた加圧ガスの残圧を抜く際には、調圧弁３をガスが逆流する必要があるが、一般的に調圧弁３はその構造上、入口圧が出口圧よりも低いときは弁が全開状態となるので、ガスの逆流が可能である。 The standard sample introduction procedure in the present embodiment is almost the same as that in the first embodiment. However, when the pressure of the pressurized gas is set by the flow rate control valve 21, the control flow of the pressure regulating valve 3 is anticipated to send the liquid. The point that should be set to a pressure slightly higher than the optimum pressure is different from the case of the first embodiment.
Further, when the residual pressure of the stored pressurized gas is released after the tuning is completed, it is necessary for the gas to flow back through the pressure regulating valve 3. Generally, the pressure regulating valve 3 is structured so that the inlet pressure is the outlet pressure. When the pressure is lower than that, the valve is fully opened, so that the gas can flow backward.

なお、上記の実施例１および２における２方電磁弁６は、電磁弁に限らず流路をオン−オフ的に開閉する他のタイプの弁で置き換えることができる。
また、２方電磁弁６以降の加圧ガス流路の内容積（液面上空間Ａの容積を含む）を大きくすれば送液精度が向上し、送液可能な時間を延ばすこともできるから、この部分の流路中に適当な容積を持つ蓄圧タンクを設けるように構成してもよい。 The two-way solenoid valve 6 in the first and second embodiments is not limited to the solenoid valve, and can be replaced with another type of valve that opens and closes the flow path on and off.
Also, if the internal volume of the pressurized gas flow path after the two-way solenoid valve 6 (including the volume of the space A above the liquid surface) is increased, the liquid feeding accuracy can be improved and the time during which the liquid can be fed can be extended. The pressure accumulating tank having an appropriate volume may be provided in the flow path of this portion.

本発明はＬＣ／ＭＳに利用できる。   The present invention can be used for LC / MS.

本発明の一実施例を示す図である。It is a figure which shows one Example of this invention. 本発明の他の実施例を示す図である。It is a figure which shows the other Example of this invention. 従来の構成例を示す図である。It is a figure which shows the example of a conventional structure.

符号の説明Explanation of symbols

１ ガス源
２ ガスコントロール部
３ 調圧弁
４ ３方電磁弁
５ 標準試料容器
６ ２方電磁弁
７ 安全弁
２１ 流量制御弁
２２ 圧力ゲージ
２３ 流路抵抗
５１ 加圧管
５２ 送液管
５３ 標準試料
Ａ 液面上空間
DESCRIPTION OF SYMBOLS 1 Gas source 2 Gas control part 3 Pressure regulating valve 4 Three-way solenoid valve 5 Standard sample container 6 Two-way solenoid valve 7 Safety valve 21 Flow control valve 22 Pressure gauge 23 Flow path resistance 51 Pressurizing pipe 52 Liquid feeding pipe 53 Standard sample A Liquid surface Upper space

Claims (2)

液体クロマトグラフ部と質量分析部が大気圧イオン化インターフェイス部を介して連結されて構成され、ガス源から流量制御弁を通して前記大気圧イオン化インターフェイス部にガスを供給するガス供給流路を有すると共に、チューニング時には液体を収めた標準試料容器内の液面上空間に連通する加圧管を通して加圧ガスを前記液面上空間に導入することにより前記標準試料の液面下に連通する送液管から前記標準試料を前記大気圧イオン化インターフェイス部に向けて送給するように構成された液体クロマトグラフ質量分析装置において、前記加圧ガスの流路が、前記流量制御弁の下流側で前記ガス供給流路から分岐され、開閉弁を介して前記加圧管に通じるように構成されていることを特徴とする液体クロマトグラフ質量分析装置。 A liquid chromatograph unit and a mass spectrometer unit are connected via an atmospheric pressure ionization interface unit, and have a gas supply channel for supplying gas from the gas source to the atmospheric pressure ionization interface unit through a flow rate control valve, and tuning. In some cases, the standard is removed from the liquid supply pipe communicating with the liquid under the liquid surface of the standard sample by introducing a pressurized gas into the liquid surface through a pressure pipe communicating with the liquid upper space in the standard sample container containing the liquid. In the liquid chromatograph mass spectrometer configured to feed the sample toward the atmospheric pressure ionization interface unit, the flow path of the pressurized gas is connected to the gas supply flow path downstream of the flow control valve. A liquid chromatograph mass spectrometer characterized in that it is branched and communicates with the pressurizing tube through an on-off valve. 入口側の圧力が出口側の圧力よりも高いときは出口側の圧力を所定圧に調圧し入口側の圧力が出口側の圧力よりも低いときは弁が全開状態となる調圧弁を、前記開閉弁と前記加圧管との間の前記加圧ガスの流路中に設けることを特徴とする請求項１に記載の液体クロマトグラフ質量分析装置。
When the pressure on the inlet side is higher than the pressure on the outlet side, the pressure on the outlet side is regulated to a predetermined pressure, and when the pressure on the inlet side is lower than the pressure on the outlet side, the pressure regulating valve is fully opened. The liquid chromatograph mass spectrometer according to claim 1, wherein the liquid chromatograph mass spectrometer is provided in a flow path of the pressurized gas between a valve and the pressurized pipe.
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