CN111089908A - Internal standard substance for retention time alignment/correction, internal standard solution, method and kit - Google Patents
Internal standard substance for retention time alignment/correction, internal standard solution, method and kit Download PDFInfo
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- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The application discloses an internal standard substance, an internal standard solution, a method and a kit for retention time alignment/correction; wherein the internal standard substance is at least one selected from 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol and 2, 4-di-tert-butylphenol. The retention time alignment/correction method is simple and easy to control in operation process and dispersed in retention time.
Description
Technical Field
The application relates to an internal standard substance, an internal standard solution, a method and a kit for retention time alignment/correction, belonging to the field of analytical chemistry.
Background
Biological big data analysis such as omics, bioinformatics and the like needs to obtain biological relevant findings through a large amount of even massive data. Experimental results typically vary from experiment to experiment and from experiment to experiment. Generally, the inter-experimental variation is of a higher magnitude than the intra-experimental variation.
In the analysis and detection process, due to the influence of various factors, the original chromatogram is easy to generate spectrum peak drift and some system bias. These errors are largely due to the influence of the column itself (column aging, packing non-uniformity, residual contaminants in the column, etc.). Even if the experimental conditions are completely parallel, these errors are difficult to avoid; even with the same experimental conditions and samples, differences can arise from changing chromatographic columns. Secondly, the difficulty in controlling some experimental conditions (temperature, elution gradient, etc.) is also one of the main causes of chromatographic retention time bias. In addition, instrument errors (dead volume, flow rate changes, baseline drift, etc.) can also have a large effect on retention time. The spectrum peak drift makes the spectrogram complex, and brings difficulties to analysis such as compound attribution, quantification, pattern recognition, data mining and the like. Therefore, the alignment and correction of the retention time of the spectrum peak become a key step in the pretreatment process of biological big data analysis. The LC-MS spectrogram alignment and correction not only can eliminate chromatographic separation analysis errors among experiments, but also can simultaneously compare LC-MS results generated in different laboratories at different times.
Biological samples (blood plasma, urine, traditional Chinese medicine extracts, compound preparations and the like) are taken as a typical complex system, and chemical components are extremely complex. The physical and chemical properties of a plurality of components are different, and the content difference is huge. In the experiment, the chromatographic retention of the compounds with different properties is affected differently by various experimental factors. The difference in polarity between the components is such that their retention time covers the entire chromatographic separation process. The sample to be analyzed in the actual analysis may not have the common compound or the chromatographic retention time of the common compound is not sufficiently dispersed. At present, no commercial retention time internal standard kit for the negative ion mode of the LC-MS exists.
Disclosure of Invention
According to one aspect of the present application, there is provided an internal standard substance for retention time alignment/correction and an internal standard liquid which are effective for chromatographic retention time alignment/correction in a negative ion mode of a LC-MS.
Specifically, substances with significant differences in polarity and stepwise increases in chromatographic retention time are used as retention time internal standards in the present application.
The invention aims to overcome the defects of the prior art and provides a retention time internal standard composition, a method and a kit for a negative ion mode of a liquid chromatograph-mass spectrometer. The internal standard substances can be used for accurately and conveniently aligning/correcting the data of the negative ion mode of the LC-MS.
The internal standard substance for retention time alignment/correction is characterized by containing at least one of 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol, and 2, 4-di-tert-butylphenol.
Optionally, the internal standard comprises 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol, and 2, 4-di-tert-butylphenol.
In another aspect of the present application, there is provided an internal standard solution for retention time alignment/correction, characterized by containing at least one of the above-mentioned internal standards.
Optionally, the time-retention alignment/correction internal standard solution comprises an internal standard; wherein the internal standard substance is at least one selected from 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol and 2, 4-di-tert-butylphenol.
Optionally, the time-retention alignment/correction internal standard solution comprises an internal standard; wherein the internal standard comprises 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol, and 2, 4-di-tert-butylphenol.
Optionally, the internal standard solution further comprises a solvent; wherein the solvent dissolves the internal standard.
Alternatively, any suitable solvent may be used as the solvent.
Optionally, the solvent comprises at least one of acetonitrile, water, methanol, ethanol.
Optionally, the solvent is selected from at least one of acetonitrile, water, methanol, ethanol.
Optionally, the solvent is a mixture obtained by mixing at least two of acetonitrile, water, methanol and ethanol in any proportion.
Alternatively, the solvent is selected from a mixture of acetonitrile and water in any ratio.
Optionally, the solvent comprises a mixture of acetonitrile and water.
Specifically, the internal standard solution comprises an internal standard substance with a predetermined concentration; and a solvent for dissolving the internal standard. The predetermined concentration is the concentration of the internal standard substance in the internal standard solution.
Optionally, the concentration of 4-tert-butylphenol in the internal standard solution is the highest concentration.
Optionally, the concentration of the intermediate nitrophenol in the internal standard solution is the lowest concentration.
Alternatively, the concentration of the internal standard solution can be adaptively selected by one skilled in the art based on the particular sample being evaluated.
Optionally, the internal standard substance and/or internal standard liquid is used in a mass spectrometer and/or a liquid chromatograph.
Optionally, the internal standard and/or internal standard liquid is used in negative ionization mode.
Optionally, the mass spectrometer is an electrospray mass spectrometer.
In particular, the internal standard substance and/or internal standard liquid is used for, but not limited to, an electrospray mass spectrometer.
In another aspect of the present application, there is provided a method for time-retention alignment/correction, which is characterized by using at least one of the above-mentioned internal standard substance for time-retention alignment/correction and the above-mentioned internal standard solution for time-retention alignment/correction.
Optionally, the method is used for retention time alignment/correction in liquid chromatography-tandem mass spectrometry.
Optionally, the method is used for retention time alignment/correction of negative ion mode of a LC-MS.
Optionally, the method comprises:
(1) obtaining a sample to be analyzed;
(2) mixing the internal standard solution with the sample to be analyzed in the step (1) to obtain a sample to be analyzed;
(3) adding the sample to be tested in the step (2) into a testing instrument to obtain a liquid chromatography-mass spectrometry chromatogram of the sample to be tested;
(4) extracting an EIC chromatogram of an internal standard substance in a sample to be detected, and determining the retention time of each internal standard substance;
(5) retention time alignment/correction is performed.
Optionally, the sample to be analyzed in step (1) is a biological sample.
Optionally, the sample to be analyzed in step (1) includes at least one of plasma, serum, cerebrospinal fluid, urine, raw traditional Chinese medicine materials, different parts of traditional Chinese medicine, and processed product of traditional Chinese medicine.
Optionally, the processed product of the traditional Chinese medicine comprises at least one of decoction pieces, powder and preparations.
Specifically, the sample to be analyzed in step (1) includes, but is not limited to, plasma, serum, cerebrospinal fluid, urine, raw traditional Chinese medicine materials, decoction pieces, powder, preparations (traditional Chinese medicine granules, traditional Chinese medicine injection, etc.), and also includes, but is not limited to, different parts of traditional Chinese medicine and various processed products thereof, and the like.
Optionally, the EIC chromatogram of the internal standard in step (4) is selected from at least one of the EIC chromatograms of m/z-129.0110, 169.0126,153.0191,138.0186,149.0963, 205.1593.
Optionally, the EIC chromatogram of the internal standard in step (4) is selected from the EIC chromatograms of m/z ═ 129.0110,169.0126,153.0191,138.0186,149.0963, 205.1593.
Optionally, step (5) comprises: chromatographic peak alignment or correction.
Optionally, the method of chromatographic peak alignment or correction comprises: a correlation optimization disentangling method, a spectrum sorting algorithm, distance and spectrum correlation optimization alignment, a multi-scale spectrum peak alignment algorithm, a spectrum peak alignment algorithm based on an empirical Bayes model and the like.
Optionally, the method comprises:
a. obtaining a sample to be analyzed;
b. adding the internal standard solution into a sample to be analyzed, and fully mixing to obtain a sample to be detected;
the internal standard solution contains an internal standard substance and a solvent for dissolving the internal standard substance;
c. injecting a sample to be detected into a liquid chromatography-mass spectrometer, and separating by a chromatographic column to obtain a liquid chromatography-mass spectrometer chromatogram of the sample to be detected;
d. extracting an EIC chromatogram of a sample to be detected, wherein m/z is 129.0110,169.0126,153.0191,138.0186,149.0963,205.1593, and determining the retention time of each internal standard substance;
e. retention time alignment/correction is performed.
As a specific embodiment, the method comprises:
a1, preparing a sample to be analyzed according to a certain preparation method;
b1, adding a certain volume of internal standard substance into the sample to be analyzed, and fully mixing to obtain the sample to be detected. The internal standard contains a plurality of known compounds and a solvent for dissolving the internal standard;
c1, injecting the sample to be detected into the LC-MS, and separating by a chromatographic column to obtain the LC-MS chromatogram of the sample to be detected;
d1, extracting an EIC chromatogram of the sample to be detected, wherein m/z is 129.0110,169.0126,153.0191,138.0186,149.0963,205.1593, and determining the retention time of each internal standard substance;
e1, performing retention time alignment/correction according to experimental requirements.
Optionally, the internal standard substance for retention time alignment/correction described above and any one of the internal standard liquids for retention time alignment/correction described above are used for a liquid chromatograph and/or a mass spectrometer.
In another aspect of the present application, there is provided the above-mentioned internal standard substance for retention time alignment/correction and/or any one of the above-mentioned internal standard liquid for retention time alignment/correction and/or any one of the above-mentioned methods for retention time alignment/correction in a negative ion mode of a mass spectrometer.
In yet another aspect of the present application, there is provided a kit characterized by comprising an internal standard and a solvent;
wherein the internal standard substance comprises at least one of 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol, and 2, 4-di-tert-butylphenol;
the solvent comprises at least one of acetonitrile, methanol, ethanol and water.
Optionally, the solvent comprises a mixture of acetonitrile and water.
Optionally, the internal standard comprises 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol, and 2, 4-di-tert-butylphenol.
Optionally, the solvent is selected from at least one of acetonitrile, methanol, ethanol, water.
Optionally, the kit of any of the above for retention time alignment/correction.
Optionally, the kit is a retention time internal standard kit for the negative ion mode of a LC-MS.
As a specific embodiment, the retention time internal standard kit for the negative ion mode of the lc comprises an internal standard substance with a predetermined concentration and a solvent for dissolving the internal standard substance.
The invention provides a retention time internal standard solution, a method and a kit for a negative ion mode of a liquid chromatograph-mass spectrometer, which comprise an internal standard substance with a preset concentration and a solvent for dissolving a composition, wherein the composition comprises 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol and 2, 4-di-tert-butylphenol. The internal standard liquid is used in the negative ionization mode of biological samples and can be used in, but is not limited to, electrospray mass spectrometers. The internal standard solution may comprise a mixture that enables alignment/calibration over a wide range of retention times.
In the application, the term "liquid chromatography-mass spectrometry" refers to a liquid chromatography-mass spectrometry technology, which uses liquid chromatography as a separation system and mass spectrometry as a detection system.
The beneficial effects that this application can produce include:
(1) retention time internal standard kits for use in LC-MS anion mode retention time alignment/correction are provided herein and are commercially available.
(2) The kit is environment-friendly, safe, practical, simple in configuration, easy to store and capable of effectively aligning/correcting the retention time of the chromatogram in the negative ion mode of the LC-MS.
(3) The method is simple and easy to control in the operation process, and the retention time is dispersed.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
The raw materials in the examples of the present application were all purchased commercially, unless otherwise specified. Wherein, the purchase sources of the 5-fluorouracil, the gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol and the 2, 4-di-tert-butylphenol reference substances are as follows: beijing Wanjia first Biotechnology Ltd.
According to one embodiment of the present application, a retention time internal standard composition for negative ion mode of a LC-MS comprises: an internal standard at a predetermined concentration; and a solvent for dissolving the internal standard.
Optionally, the internal standard is used in a liquid chromatograph.
Optionally, the internal standard is used in a mass spectrometer.
Optionally, the internal standard is used in negative ionization mode.
Optionally, the internal standard is used in, but not limited to, an electrospray mass spectrometer.
Optionally, the internal standard comprises 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol, 2, 4-di-tert-butylphenol.
Optionally, the solvent in which the internal standard is dissolved comprises a mixture of acetonitrile and water.
According to one embodiment of the application, a method for using an internal standard of retention time for negative ion mode of a liquid chromatograph-mass spectrometer adopts the composition of any one of the above items, and specifically comprises the following steps:
(1) preparing a sample to be analyzed according to a certain preparation method
(2) And adding the internal standard substance with a certain volume into the sample to be analyzed, and fully mixing to obtain the sample to be detected. The internal standard contains a plurality of known compounds and a solvent for dissolving the internal standard;
(3) injecting a sample to be detected into a liquid chromatography-mass spectrometer, and separating by a chromatographic column to obtain a liquid chromatography-mass spectrometer chromatogram of the sample to be detected;
(4) extracting an EIC chromatogram of a sample to be detected, wherein m/z is 129.0110,169.0126,153.0191,138.0186,149.0963,205.1593, and determining the retention time of each internal standard substance;
(5) retention time alignment/correction is performed according to experimental requirements.
Optionally, the internal standard is used in a liquid chromatograph.
Optionally, the internal standard is used in a mass spectrometer.
Optionally, the internal standard is used in negative ionization mode.
Optionally, the internal standard is used in, but not limited to, an electrospray mass spectrometer.
Optionally, the internal standard comprises 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol, 2, 4-di-tert-butylphenol.
Optionally, the solvent in which the internal standard is dissolved comprises a mixture of acetonitrile and water.
According to one embodiment of the present application, a retention time internal standard kit for negative ion mode of a LC-MS comprises: an internal standard at a predetermined concentration; and a solvent for dissolving the composition.
Optionally, the internal standard is used in a liquid chromatograph.
Optionally, the internal standard is used in a mass spectrometer.
The retention time internal standard kit for the negative ion mode of the LC-MS is characterized by comprising the following components in parts by weight: the internal standard was used in negative ionization mode.
Optionally, the internal standard is used in, but not limited to, an electrospray mass spectrometer.
Optionally, the internal standard comprises 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol, 2, 4-di-tert-butylphenol.
Optionally, the solvent in which the internal standard is dissolved comprises a mixture of acetonitrile and water.
Example 1
1. Preparation of the sample to be analyzed.
In this example, ligusticum wallichii (1; sample number n is 23), ledebouriella root (2; sample number n is 24), bupleurum root (3; sample number n is 22), notopterygium root (4; sample number n is 21), cnidium fruit (5; sample number n is 21), angelica sinensis (6; sample number n is 21), angelica dahurica (7; sample number n is 22), ligusticum (8; sample number n is 22), fennel (9; sample number n is 22), 100mg of each powder of the traditional Chinese medicine samples are taken, methanol with a volume concentration of 50% is added respectively, 0.5ml is added, ultrasonic extraction is carried out for 10min, supernatant is taken after high-speed centrifugation at 15000 rpm for 10min, 0.5ml methanol with a volume concentration of 50% is added again into filter residues, ultrasonic extraction is carried out for 10min, and supernatant is taken after high-speed centrifugation at 15000 rpm for 10 min. Mixing the two extractive solutions to obtain supernatant.
2. Adding 10ul of internal standard solution into 40ul of samples to be analyzed, and fully mixing to obtain samples to be detected; the internal standard substance contains 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol, 2, 4-di-tert-butylphenol and a solvent for dissolving the internal standard substance;
wherein, the specific composition of 10ul internal standard solution is as follows: weighing a proper amount of 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol and 2, 4-di-tert-butylphenol as reference substances, and adding an acetonitrile-water mixed solution (the volume ratio of acetonitrile to water is 70:30) to prepare internal standard stock solutions with the mass concentrations of 10mg/mL, 1mg/mL, 0.3mg/mL, 50mg/mL and 33.33mg/mL respectively. 100ul of each internal standard mother liquor is taken to prepare mixed internal standard solution.
3. Acquisition of negative ion mode data of to-be-detected sample LC-MS
An Agilent 1290 ultra performance liquid chromatography system (Agilent, Waldbronn, Germany) was used in this example in tandem with 6520Q-TOF-MS (Agilent Corp, USA).
(1) Chromatographic methods in this example, a ZORBAX Eclipse Plus C18 chromatographic column (3.0X 150mm,1.8um) from Agilent corporation was used, mobile phase A was water (0.2% formic acid), phase B was acetonitrile, gradient elution: 0-15min, 5% -100% of phase B, and flow rate of 0.4 ml/min. The column temperature was 60 ℃ and the sample size was 5 uL.
Wherein, the percentages of the substances are volume percentages.
(2) Mass spectrometry method
In the embodiment, the mass spectrum adopts an ESI ion source and acquires data in a negative ion mode. The data acquisition range is m/z 100-. The temperature is 350 ℃, the flow rate of the dryer is 8L/min, the pressure of the atomization gas is 40psi, the voltage of the capillary tube is 3500V, the fragmentation voltage is 175V, and the voltage of the taper hole is 65V.
4. EIC chromatogram of sample m/z 129.0110,169.0126,153.0191,138.0186,149.0963,205.1593 is extracted, retention time of each internal standard substance is determined, and table 1 shows
Wherein, table 1 is a list of retention times of nine traditional Chinese medicine internal standard substances in example 1.
5. Perform retention time alignment/correction: the UM-1-001 sample reference sample is designated in QI software, the coordinates of 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol and 2, 4-di-tert-butylphenol are manually marked, and a peak alignment program is run.
As can be seen from the above, this approach achieves the desired retention time alignment/correction.
In Table 1, "-" indicates no detection.
Other biological samples described in this application may be aligned/corrected for retention time using the methods described above.
TABLE 1
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. An internal standard substance for retention time alignment/correction, characterized by comprising at least one of 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol, and 2, 4-di-tert-butylphenol.
2. An internal standard according to claim 1, wherein the internal standard comprises 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol, and 2, 4-di-tert-butylphenol.
3. An internal standard solution for retention time alignment/correction, comprising at least one of the internal standards according to claim 1 or 2;
preferably, the internal standard solution further comprises a solvent; wherein the solvent dissolves the internal standard;
preferably, the solvent comprises at least one of acetonitrile, methanol, ethanol, water.
4. A method for time-retention alignment/correction, characterized by using at least one of the internal standard for time-retention alignment/correction according to claim 1 or 2 and the internal standard liquid for time-retention alignment/correction according to claim 3.
5. The method of claim 4, wherein the method is used for retention time alignment/correction in LC-MS;
preferably, the method is used for retention time alignment/correction of negative ion mode of LC-MS;
preferably, the method comprises:
(1) obtaining a sample to be analyzed;
(2) mixing the internal standard solution with the sample to be analyzed in the step (1) to obtain a sample to be analyzed;
(3) adding the sample to be tested in the step (2) into a testing instrument to obtain a liquid chromatography-mass spectrometry chromatogram of the sample to be tested;
(4) extracting an EIC chromatogram of an internal standard substance in a sample to be detected, and determining the retention time of each internal standard substance;
(5) performing retention time alignment/correction;
preferably, the EIC chromatogram of the internal standard in step (4) is selected from at least one of the EIC chromatograms of m/z-129.0110, 169.0126,153.0191,138.0186,149.0963, 205.1593;
preferably, the EIC chromatogram of said internal standard in step (4) is selected from the EIC chromatograms of m/z ═ 129.0110,169.0126,153.0191,138.0186,149.0963, 205.1593;
preferably, the method comprises:
a. obtaining a sample to be analyzed;
b. adding the internal standard solution into a sample to be analyzed, and fully mixing to obtain a sample to be detected;
the internal standard solution contains an internal standard substance and a solvent for dissolving the internal standard substance;
c. injecting a sample to be detected into a liquid chromatography-mass spectrometer, and separating by a chromatographic column to obtain a liquid chromatography-mass spectrometer chromatogram of the sample to be detected;
d. extracting an EIC chromatogram of a sample to be detected, wherein m/z is 129.0110,169.0126,153.0191,138.0186,149.0963,205.1593, and determining the retention time of each internal standard substance;
e. retention time alignment/correction is performed.
6. The internal standard substance for retention time alignment/correction described in claim 1 or 2, and the internal standard liquid for retention time alignment/correction described in claim 3 are used for a liquid chromatograph and/or a mass spectrometer.
7. The use of the internal standard substance for retention time alignment/correction according to claim 1 or 2 and/or the internal standard liquid for retention time alignment/correction according to claim 3 and/or the method for retention time alignment/correction according to claim 4 or 5 for retention time alignment/correction of a negative ion mode of a LC-MS.
8. A kit comprising an internal standard and a solvent;
wherein the internal standard substance comprises at least one of 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol, and 2, 4-di-tert-butylphenol;
the solvent comprises at least one of acetonitrile, methanol, ethanol and water.
9. The kit of claim 8, wherein the internal standard comprises 5-fluorouracil, gallic acid, protocatechuic acid, m-nitrophenol, 4-tert-butylphenol, and 2, 4-di-tert-butylphenol;
preferably, the solvent is selected from at least one of acetonitrile, methanol, ethanol, water.
10. The kit of claim 8 or 9 for retention time alignment/correction.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1146062B1 (en) * | 2000-04-12 | 2006-12-20 | Kaneka Corporation | Method of producing crosslinkable silyl group-containing polyoxyalkylene polymers |
| CN102759584A (en) * | 2012-06-20 | 2012-10-31 | 遵义林源医药化工有限责任公司 | Method for determining pyrogallic acid through high performance liquid chromatography |
| CN103018317A (en) * | 2013-01-04 | 2013-04-03 | 中国药科大学 | Novel non-standard-dependence quantitative analysis method based on study on homologous/similar compound structure-mass-spectrum response relationship |
| JP2015518499A (en) * | 2012-03-28 | 2015-07-02 | テューリンギッシェス・インスティトゥート・フューア・テクスティル−ウント・クンストストッフ−フォルシュング・エー・ファウ | Multifunctional coating film that can be applied in liquid form |
| CN105259268A (en) * | 2015-10-30 | 2016-01-20 | 上海杏灵科技药业股份有限公司 | Detection method for fingerprint chromatogram of flavonoid and organic acid components in ginkgo biloba extract and application of detection method |
| US20170196869A1 (en) * | 2015-12-09 | 2017-07-13 | Expression Pathology, Inc. | Methods for treating Her2-positive breast cancer |
| CN108593825A (en) * | 2018-01-24 | 2018-09-28 | 中国科学院大连化学物理研究所 | The excavation of red ginseng mass spectrometric data and the screening technique of Specific marker |
-
2018
- 2018-10-24 CN CN201811241715.0A patent/CN111089908A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1146062B1 (en) * | 2000-04-12 | 2006-12-20 | Kaneka Corporation | Method of producing crosslinkable silyl group-containing polyoxyalkylene polymers |
| JP2015518499A (en) * | 2012-03-28 | 2015-07-02 | テューリンギッシェス・インスティトゥート・フューア・テクスティル−ウント・クンストストッフ−フォルシュング・エー・ファウ | Multifunctional coating film that can be applied in liquid form |
| CN102759584A (en) * | 2012-06-20 | 2012-10-31 | 遵义林源医药化工有限责任公司 | Method for determining pyrogallic acid through high performance liquid chromatography |
| CN103018317A (en) * | 2013-01-04 | 2013-04-03 | 中国药科大学 | Novel non-standard-dependence quantitative analysis method based on study on homologous/similar compound structure-mass-spectrum response relationship |
| CN105259268A (en) * | 2015-10-30 | 2016-01-20 | 上海杏灵科技药业股份有限公司 | Detection method for fingerprint chromatogram of flavonoid and organic acid components in ginkgo biloba extract and application of detection method |
| US20170196869A1 (en) * | 2015-12-09 | 2017-07-13 | Expression Pathology, Inc. | Methods for treating Her2-positive breast cancer |
| CN108593825A (en) * | 2018-01-24 | 2018-09-28 | 中国科学院大连化学物理研究所 | The excavation of red ginseng mass spectrometric data and the screening technique of Specific marker |
Non-Patent Citations (4)
| Title |
|---|
| QIANG ZHAO 等: "Rapid discrimination between red and white ginseng based on uniqueunique mass-spectrometric features", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》 * |
| YU YIN 等: "Biological Activities of Water and Ethanol Extracts from Two Varieties of Rubus coreanus Miquel Fruits", 《JOURNAL OF FOOD SCIENCE AND NUTRITION》 * |
| 刘艳纯 等: "钩吻中非生物碱化学成分的研究进展", 《中国兽药杂志》 * |
| 时圣明 等: "虎杖的化学成分及药理作用研究进展", 《药物评价研究》 * |
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