Shimadzu Corporation

Kobe University

Shuichi Kawana

Manabu Shimomura

Katsuyuki Taneda

Kazuo Mukaibatake

Shiro Mizutani

Yukihiko Kudo

Noriyuki Ojima

Takero Sakai

Kenichi Obayashi

Takeshi Azuma

Masaru Yoshida

Shin Nishiumi

Yumi Unno

Takashi Kobayashi

At least one stable isotope reagent is added to each biological sample and standard sample to prepare biological samples for analysis and standard sample for analysis. The quality of the biological samples is evaluated using data of one set of biological samples for analysis composed of a plurality of biological samples for analysis. Besides, the quality of a pretreatment and/or analysis of each set of samples for analysis is evaluated using data obtained by analyzing the standard sample for analysis before and after an analysis of one set of samples for analysis. An abnormality in a chromatograph or mass analyzer used for the analysis of one set of samples is evaluated by the data obtained by analyzing a sample for device evaluation before and after the analysis of one set of samples for analysis. Thus, the quality of data obtained by chromatographic mass spectrometry on biological samples is comprehensively evaluated.

Method and device for chromatographic mass spectrometry

A measurement EIC for quantitative ions and a measurement EIC for ions to be confirmed in the vicinity of the retention time of a target compound are displayed in an overlapping manner in a chromatogram display area. In addition, a standard center line corresponding to a standard value of the confirmation ion ratio, which expresses the ratio of the intensity of the confirmation ions to the intensity of the quantitative ions in the target compound and an upper limit line and a lower limit line demonstrating the permissible range of the intensity of the confirmation ions are displayed in an overlapping manner on the EIC. An analyst determines whether a peak used for identification originates from the target compound by determining whether the top of an EIC peak of the confirmation ions falls between the upper limit line and the lower limit line.

Chromatograph mass spectrometry data processing device

A gas chromatograph having a column which separates respective components contained in a gas sample introduced via a carrier gas over time, wherein an analysis mode and a standby mode can be switched and executed. The gas chromatograph apparatus comprises: a carrier gas flow path, a column protection gas flow path, a flow path switching part provided between the carrier gas flow path and the column protection gas flow path and a column so that only one of the carrier gas or a column protection gas is introduced into the column, and a flow path control part for controlling the flow switching part so as to introduce the carrier gas into the column at the time of the analysis mode and introduce the column protection gas into the column at the time of the standby mode.

Gas chromatograph apparatus

A gas chromatograph mass spectrometer including: an oven for gas chromatography, a mass spectrometry part, a sample vaporization chamber, a gas supply part, and a control part. When the replacement operation of a septum or a glass insert begins, the control part controls the gas supply part so that the flow rate of a carrier gas has a constant pressure and then controls heaters so that temperature is equal to or less than a temperature at which replacement is possible. When temperature becomes equal to or less than the temperature at which replacement is possible and the replacement operation of the septum or the glass insert is completed, the control part controls the heaters so that the temperature is an analysis temperature and controls the gas supply part to employ the same control method for the flow rate of the carrier gas as that before the replacement operation is begun.

Gas chromatograph mass spectrometer

Disclosed is a quadrupole mass spectrometer, which is capable of, during an SIM measurement, maximally reducing a settling time-period necessary for an operation of changing an input voltage to a quadrupole mass filter in a staircase pattern, and preventing unwanted ions from excessively entering a detector during a course of changing between a plurality of mass values. Under a condition that a response speed of a DC voltage U to be applied to quadrupole electrodes is less than that of an amplitude of a high-frequency voltage V, a control sectionis operable to rearrange the mass values in descending order of mass value, and an optimal settling-time calculation sub-sectionis operable to determine a settling time-period for each of the mass values, based on a mass-value difference and a post-change mass value.

Quadrupole mass spectrometer including voltage variable DC and amplitude variable AC for selected ion monitoring / scan alternate measurement

Disclosed is a quadrupole mass spectrometer, which is capable of, during an SIM measurement, maximally reducing a settling time-period necessary for an operation of changing an input voltage to a quadrupole mass filter in a staircase pattern, and preventing unwanted ions from excessively entering a detector during a course of changing between a plurality of mass values. Under a condition that a response speed of a DC voltage U to be applied to quadrupole electrodes is less than that of an amplitude of a high-frequency voltage V, a control section 10 is operable to rearrange the mass values in descending order of mass value, and an optimal settling-time calculation sub-section 101 is operable to determine a settling time-period for each of the mass values, based on a mass-value difference and a post-change mass value.

Quadrupole mass spectrometer including voltage variable DC and amplitude variable AC

The present invention aims at realizing an energy-saving mode in which the usage of a carrier gas and the power consumption are sufficiently suppressed without causing damage to the apparatus. When a command for executing the energy-saving mode is entered (S), the column flow rate after the transition to the energy-saving mode (when the temperature decreases) is computed by using control parameters determined in correspondence to the energy-saving mode. If the flow rate exceeds the allowable upper limit determined by the configuration of the apparatus (Sand S), a warning for urging users to decrease the column inlet pressure and enter the command again is displayed (S). If the computed flow rate is not higher than the allowable upper limit, a constant pressure control is performed aiming at the inlet pressure at that point in time (Sand S). Although the column flow rate gradually increases after the heater of the column oven is turned off, it will not exceed the allowable upper limit. Thus, the detector is prevented from being damaged.

A table () for relating an appropriate DC bias voltage to each of a plurality of selectable scan speeds is stored beforehand in an auto-tuning data memory section (). In an auto-tuning operation, a controller () determines the DC bias voltage corresponding to each scan speed by referring to the table () and fixes the output of an ion-drawing voltage generator () at that voltage. Subsequently, while changing the voltages applied to relevant sections such as an ion optical system (), the controller () finds voltage conditions under which the detection signal is maximized. The conditions thus found are stored in an auto-tuning result data (). In an analysis of a target sample, a DC bias voltage corresponding to a scan speed specified by an operator is obtained from the DC bias voltage table (), and the optimal conditions for this voltage are obtained from the auto-tuning result data (). Based on these items of information, conditions for the scan measurement are determined. This method prevents the deterioration in detection sensitivity, which will otherwise take place if the scan measurement is performed at a high scan speed.

Quadrupole mass spectrometer

An electrically conductive heat-blocking platewith an openingfor allowing thermions to pass through is provided between a filamentwhose temperature can be as high as 2000&#xb0; to 3000&#xb0; C., and an ionization chamber. The heat-blocking plateis thermally connected via an aluminum blockto a heater for maintaining the ionization chamberwithin a range temperature from 200&#xb0; to 300&#xb0; C., and also electrically set at a ground potential, which is approximately equal to the potential of the ionization chamberThe heat-blocking plateblocks the radiation heat that the filamentemits when energized. Thus, the wall of the ionization chamberis prevented from being locally heated to an abnormally high temperature. As a result, the inner space of the ionization chamberis maintained at an approximately uniform temperature, and the noise due to the decomposition of a metallic material by abnormal heating is prevented. The heat-blocking platealso prevents a thermion-accelerating electric field from penetrating through an electron injection portinto the ionization chamberand impeding the extraction of ions produced within the ionization chamber. Thus, the ion extraction efficiency is also improved.

Mass spectrometer

A gas chromatograph (GC) apparatus capable of detecting abnormality, in which a reference retention index is obtained from a result obtained by analyzing a given substance and a retention-index reference substance under adequate analysis conditions using a normal column, and stored in a storage section. Further, under a condition that the apparatus can perform normal analysis, the given substance is subjected to GC analysis to obtain a reference retention time, and the obtained reference retention time is stored in the storage section. A diagnosis processing section is operable to compare each of an actual retention time and an actual retention index with a respective one of the reference retention time and the reference retention index. If a deviation therebetween or abnormality is detected, the diagnosis processing section is operable to estimate a causal factor of the abnormality.

Gas chromatography apparatus

A quadruple mass spectrometer capable of reducing a settling time-period necessary in a process of changing, in a pulsed or step-like pattern, a voltage to be applied to a quadruple mass filter in a scan or SIM measurement. In the SIM measurement, an optimal settling-time calculation sub-section sets a length of the settling time-period according to a difference &#x394;M between a next-measurement mass value and a mass value used in an adjacent measurement, and the next-measurement mass value. This makes it possible to shorten a duration of a repetitive cycle in the SIM measurement or increase a time-period assignable to a measurement operation, while ensuring a voltage stabilization time-period sufficient to detect ions having the next-measurement mass value.

A filamentfor generating thermions is remotely located from an ionization chamberso that a thermion-accelerating electric field created by a potential difference between the filamentand the ionization chamberis prevented from penetrating through an electron injection portinto the ionization chamber. This design eliminates the disturbance of an ion-extracting electric field created within the ionization chamberby a voltage applied to lens electrodes, thus enabling ions produced within the ionization chamberto be efficiently extracted and transported to a mass analyzer located at the subsequent stage. As a result, the level of detection signals of a detector is increased, so that the mass analysis can be performed with high sensitivity.

An electron beam source device is provided in which the disconnection and deterioration of a filament of the electron beam source device can be accurately predicted and determined, so as to avoid an unnecessary resource waste and increase of cost due to a premature replacement of a still-functional filament in a conventional device. Additionally, disorganization caused by a sudden disconnection or by the subsequent recovery procedure when the deformation of the filament occurs can be avoided to, reduce the measuring time, the maintenance and management man-hour. A filament current is measured at all time through a filament current measuring circuit, and a ratio of the filament current when the light-on time is zero to the current filament current is calculated at all time through an operational circuit

Electron beam source device available for detecting life span of filament

A method of gas chromatograph mass spectrometry with a negative chemical ionization (NCI) process includes analyzing a standard substance for the NCI by deriving with a derivatization reagent a fatty acid with a multiple number of carbon atoms, measuring the standard substance for the NCI by negative chemical ionization, and obtaining a retention time for each of the number of carbon atoms. The method includes measuring, under a same condition, a standard sample of each of from one to a plurality of measurement object components by negative chemical ionization, and obtaining a respective retention time for each of the measurement object components, and obtaining a retention index for the NCI of each measurement object component using the respective retention time of the measurement object component, and the retention time of the standard substance. The index facilitates both correcting the retention time of each measurement object component, and identifying substances.

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Kyoto, Japan

Shuichi Kawana