CN111983044A - Detection method for analyzing steroid hormone based on double-derivative treatment - Google Patents
Detection method for analyzing steroid hormone based on double-derivative treatment Download PDFInfo
- Publication number
- CN111983044A CN111983044A CN201910443241.6A CN201910443241A CN111983044A CN 111983044 A CN111983044 A CN 111983044A CN 201910443241 A CN201910443241 A CN 201910443241A CN 111983044 A CN111983044 A CN 111983044A
- Authority
- CN
- China
- Prior art keywords
- steroid hormone
- sample
- detection method
- derivative
- steroid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- 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
- G01N30/02—Column chromatography
-
- 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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/55—Design of synthesis routes, e.g. reducing the use of auxiliary or protecting groups
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention belongs to the technical field of analysis, and particularly relates to a detection method for analyzing steroid hormones based on double-derivative processing. According to the method, methoxyamine is used as a derivative reagent to derive the steroid hormone containing carbonyl, dansyl chloride is used to derive the steroid hormone containing phenolic hydroxyl, and the derived products are mixed and then used for liquid chromatography tandem mass spectrometry, so that the steroid hormone containing carbonyl or phenolic hydroxyl can be detected at the same time with high sensitivity, including androgen, estrogen, progestogen, cortical hormone and the like. The analysis method has the advantages of mild derivatization reaction conditions, high detection sensitivity, wide linear range and the like.
Description
Technical Field
The invention belongs to the technical field of analysis, and relates to a liquid chromatography-mass spectrometry combined detection method for analyzing steroid hormones based on double-derivative treatment, which realizes the simultaneous detection of carbonyl and phenolic hydroxyl steroid hormones in the same sample.
Background
Steroid hormones are extremely important metabolites, participate in regulating various vital activities of human bodies as signal molecules, and play a vital role in maintaining secondary sexual characteristics, regulating gene transcription, regulating endocrine, immune function and the like. At present, the detection of single or small amount of steroid hormone is widely applied in the auxiliary clinical diagnosis, however, the level of steroid hormone in human body is greatly different individually and is easily influenced by factors such as physiological cycle. Therefore, clinical diagnosis or pathological typing by detecting a single or a small amount of steroid hormones is liable to cause misjudgment. The quantitative analysis of the steroid hormone metabolome can better research the network change of the steroid hormone on the whole, and the diagnosis result obtained based on the network change is more accurate and reliable. However, due to the low content of steroid hormones in human body, it brings great difficulties and challenges to the detection of the whole network.
The detection method of steroid hormones mainly comprises immunoassay, gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS) technologies. The LC-MS method can simultaneously carry out high-sensitivity specific detection on a plurality of steroid hormones, and is an ideal technology for carrying out high-throughput analysis on the whole steroid hormone metabolic network. The chemical derivatization technology is a common sample pretreatment technology, can improve the retention capacity of a target compound on a liquid chromatographic column on one hand, and can improve the ionization efficiency of mass spectrometry on the other hand, thereby improving the detection sensitivity. It has been reported in the literature that derivatization of hydroxy groups contained in hormones is generally performed, for example, dimethylamino benzoic acid is used to derivatize steroid hormones containing hydroxy groups, a catalyst and reaction conditions at higher temperature are required, the conditions are harsh, and the derivatization reaction time is longer. Since most steroid hormones contain carbonyl groups, chromatographic retention and detection sensitivity can also be improved by derivatization of the carbonyl group with hydroxylamine and Girard's P (GP), etc., and the reaction conditions are relatively mild. However, the method omits a small amount of steroid hormones, for example, estrogen only contains phenolic hydroxyl, and the dansyl chloride derivatization method can be adopted to improve the detection sensitivity of the steroid hormones containing the phenolic hydroxyl. Aiming at the problems existing in the conventional steroid hormone detection, in order to expand the coverage range of the steroid hormone detection, the invention aims to establish a high-sensitivity method based on the double-derivation of methoxyamine and dansyl chloride combined with LC-MS (liquid chromatography-mass spectrometry) so as to realize the simultaneous analysis of steroid hormones containing carbonyl and phenolic hydroxyl.
Disclosure of Invention
Aiming at the defects of the existing method, the invention establishes a detection method for analyzing steroid hormone based on double-derivative processing, and the method not only can improve the retention and separation degree of the steroid hormone on reversed-phase liquid chromatography, but also can improve the mass spectrum detection sensitivity of the low-abundance steroid hormone. The analysis method has the advantages of mild derivatization reaction conditions, high detection sensitivity, wide linear range and the like.
The technical route adopted by the invention is as follows:
step one, serum sample collection and pretreatment: thawing the serum sample at 4 ℃, uniformly mixing by vortex, putting 50-100 mu L into a 1.5mL centrifuge tube, adding 0.5-1mL dichloromethane solution, carrying out vortex oscillation on the mixed solution on an oscillator for 3-5min, centrifuging for 10-15min at 14000rpm/min in a 4 ℃ centrifuge, finally taking 900 mu L of the lower organic layer into the 1.5mL centrifuge tube, and freeze-drying on a freeze dryer.
In the second step, methoxyamine is derived from the steroid hormones containing carbonyl group: adding 5-10 μ g of lyophilized serum sample into 45-90 μ L of 50mM methoxylamine methanol solution, vortexing for 1min, reacting in water bath at 60 deg.C for 20-40min, taking out, and standing on ice for 1 min.
Third, dansyl chloride-derived phenolic hydroxyl group-containing hormone: adding 5-30 μ L5 mg/mL dansyl chloroacetonitrile solution and 15-30 μ L0.15M Na into another part of lyophilized serum sample 5-10 μ g 2CO3/NaHCO3Swirling the aqueous solution for 1min, placing the aqueous solution in a water bath at the temperature of 60 ℃ for reaction for 20-40min, then continuously adding 15-30 mu L of butylamine aqueous solution with the concentration of 0.5mol/L, and reacting in the water bath at the temperature of 60 ℃ for 30-50 min. Taking out, and standing on ice for 1 min.
Fourthly, centrifuging two samples after derivatization treatment, and taking supernate for liquid chromatography-mass spectrometry combined analysis: and (3) centrifuging the derivative product obtained in the step (A) in a centrifuge at 4 ℃ at 14000rpm/min for 10-15min, and reserving the supernatant for detection.
And fifthly, taking 60 mu L of supernatant in the fourth step, mixing, vortexing for 1-2min, and analyzing by liquid chromatography-mass spectrometry (LC-MS) sample injection.
In addition, the improvement effect of Methoxyamine (MOA) and 2-HP on the steroid hormone detection sensitivity in the double-derivation method is compared by optimizing a derivation reagent, and the result shows that the response of a derivative product of methoxyamine is higher than that of 2-HP, because an alkaline mixed system is not beneficial to ionization of the derivative product of 2-HP, and has small influence on the derivative product of methoxyamine. Finally, selecting methoxyamine derived carbonyl-containing steroid hormone and dansyl chloride derived phenolic hydroxyl-containing steroid hormone.
The invention has the following advantages:
due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages: two different derivatization reagents, namely methoxyamine and dansyl chloride, are adopted to respectively derivatize steroid hormone containing carbonyl and steroid hormone containing phenolic hydroxyl, and the derivatized products are mixed and then used for liquid chromatography tandem mass spectrometry. Compared with the traditional single derivation method, the double derivation method can simultaneously detect the steroid hormone containing carbonyl and phenolic hydroxyl with high sensitivity, and comprises androgen, estrogen, progestogen, cortical hormone and the like. In addition, the method also has the advantages of mild derivatization reaction conditions, high detection sensitivity, wide linear range and the like.
Drawings
FIG. 1 is a schematic diagram of the reaction principle of (A) methoxyamine derived carbonyl-containing steroid hormone and (B) dansyl chloride derived phenolic hydroxyl-containing steroid hormone.
FIG. 2 is a schematic diagram of the hormone analysis scheme in serum samples (Ar: aromatic compounds; DC: dansyl chloride).
FIG. 3 MRM chromatograms of 29 steroid hormones derived from methylamine and dansyl chloride in spiked blood samples.
Detailed Description
The invention relates to a detection method for analyzing steroid hormone based on double-derivative processing, which is elaborated by specific examples.
Example 1 serum was thawed at 4 ℃ and vortexed to mix well, 100. mu.L of each was placed in 1.5mL centrifuge tubes, 1mL of dichloromethane solution was added, the mixture was vortexed on a vortexer for 5min, then centrifuged at 14000rpm/min in a 4 ℃ centrifuge for 10min, 900. mu.L of the lower organic layer was removed in 1.5mL centrifuge tubes and lyophilized in a lyophilizer. Adding 90 mu L of a 50mM methoxylamine methanol solution into 10 mu g of the freeze-dried sample a, swirling for 1min, placing in a water bath with the temperature of 60 ℃ for reaction for 30min, taking out, placing on ice and placing for 1 min. mu.L of 5mg/mL solution was added to 10. mu.g of the lyophilized sample bDansyl chloride acetonitrile solution and 30 μ L of 0.15M Na2CO3/NaHCO3Swirling the water solution for 1min, reacting in 60 deg.C water bath for 30min, adding 30 μ L of 0.5mol/L butylamine water solution, reacting in 60 deg.C water bath for 40min, taking out, and standing on ice for 1 min. The derivatized samples a and b were centrifuged at 14000rpm/min in a centrifuge at 4 ℃ for 10min, and finally, 60. mu.L of each supernatant of the samples a and b was mixed and vortexed for LC-MS sample analysis.
Example 2 detection and analysis were performed by ultra performance liquid chromatography tandem quadrupole-ion trap mass spectrometry. Liquid chromatography conditions: the separation was carried out using a BEH C18 column (10 cm. times.2.1 mm, 1.7 μm) at a column temperature of 40 ℃ and a sample size of 10. mu.L. The mobile phase was 0.1% aqueous formic acid (phase A) and 0.1% acetonitrile formate (phase B), the flow rate was 0.25mL/min, and the linear gradient was as follows: 0min, 30% B; 5min, 98% B; 8min, 98% B; 8.1min, 30% B; 10min, 30% B. Mass spectrum conditions: the air curtain air, GAS1 and GAS2 are 0.241 MPa and 0.276MPa respectively. The spray voltage is 5.5kV, the ion source temperature is 50 ℃, the sample is analyzed in a positive ion electrospray ionization mode, a multi-reaction detection mode (MRM) is adopted to analyze the sample, the MRM parameter conditions of 29 detected hormones are shown in table 1, and the linear range, R2, detection limit, quantification limit and recovery rate of 29 steroid hormones are shown in table 2.
The detection results of the examples show that the detection method for analyzing steroid hormones based on double-derivatization treatment, which is established by the invention, has the following significant advantages compared with the methods reported in the existing literature:
1) the pretreatment process is simple and quick, and the derivatization reaction condition is mild.
2) After the derivation, the detection sensitivity of 29 steroid hormones is improved by a factor of up to 1000, the minimum detection limit of the steroid hormones reaches 0.5-5pg/mL, the linear range is wide and reaches 2-4 orders of magnitude (see Table 2). At the same time, the method shows good precision, repeatability, stability and recovery.
3) The steroid hormone has high coverage, comprises four main groups of androgen, estrogen, progestogen and corticoid, and basically covers the most important hormone in the human body.
TABLE 129 MRM analysis parameters of steroid hormones
Linear range, R, of table 229 steroid hormones2Detection limit, quantitation limit, and recovery rate
Claims (6)
1. A detection method for analyzing steroid hormones based on double-derivative treatment is characterized in that: selecting methoxyamine as a derivative reagent of steroid hormone containing carbonyl, dansyl chloride as a derivative reagent of steroid hormone containing phenolic hydroxyl to treat a sample, and detecting the derivative steroid hormone by liquid chromatography-mass spectrometry to realize the simultaneous detection of the steroid hormone containing carbonyl and phenolic hydroxyl in the same sample, which specifically comprises the following steps:
firstly, collecting and pretreating a serum sample;
secondly, taking the treated sample obtained in the first step, and performing derivatization treatment on the sample, wherein the steroid hormone containing carbonyl in the sample is specifically derivatized by methoxyamine;
thirdly, taking the treated sample obtained in the first step, and performing derivatization treatment on the sample, wherein the steroid hormone containing phenolic hydroxyl is specifically derivatized by dansyl chloride;
fourthly, respectively carrying out centrifugal treatment on the two samples subjected to the derivatization treatment obtained in the second step and the third step, and reserving supernate for analysis by liquid chromatography-mass spectrometry;
And fifthly, mixing the two supernatants obtained in the fourth step, and detecting and analyzing the steroid hormones by liquid chromatography-mass spectrometry.
2. The detection method according to claim 1, characterized in that: in the first step, a serum sample is unfrozen at 4 ℃, is uniformly mixed in a vortex mode, 50-100 mu L of the mixture is placed in a 1.5mL centrifuge tube, 0.5-1mL dichloromethane solution is added, the mixture is subjected to vortex oscillation on an oscillator for 3-5min, then is centrifuged in a 4 ℃ centrifuge at the speed of 14000rpm/min for 10-15min, and finally, 450 mu L of a lower organic layer and 900 mu L of the lower organic layer are placed in the 1.5mL centrifuge tube and are freeze-dried on a freeze dryer.
3. The detection method according to claim 1 or 2, characterized in that: in the second step, the steroid hormone containing carbonyl is derived by using methoxyamine, and the derivation reaction process is as follows: and adding 5-10 mu g of the freeze-dried serum sample obtained by the first step into 45-90 mu L of a 50mM methoxylamine methanol solution, whirling for 1min, placing in a water bath with the temperature of 60 ℃ for reaction for 20-40min, taking out, placing on ice, and placing for 1min to obtain a derivative treated sample.
4. The detection method according to claim 1, characterized in that: in the third step, the steroid hormone containing the phenolic hydroxyl is derived by dansyl chloride, and the derivation reaction process is as follows: adding 5-10 μ g of lyophilized serum sample obtained from the first step into 15-30 μ L of 5mg/mL dansyl chloroacetonitrile solution and 15-30 μ L of 0.15M Na 2CO3/NaHCO3And (3) swirling the aqueous solution for 1min, placing the aqueous solution in a water bath at the temperature of 60 ℃ for reacting for 20-40min, then continuously adding 15-30 mu L of butylamine aqueous solution with the concentration of 0.5mol/L, reacting for 30-50min in the water bath at the temperature of 60 ℃, taking out the butylamine aqueous solution, placing the butylamine aqueous solution on ice for 1min to obtain a derivative treated sample.
5. The detection method according to claim 1, characterized in that: in the fourth step, the samples which are obtained in the second step and the third step and are subjected to derivatization treatment are respectively centrifuged for 10-15min in a centrifuge at the temperature of 4 ℃ at the speed of 14000rpm/min, and supernatant liquid is reserved for detection by liquid chromatography-mass spectrometry.
6. The detection method according to claim 1, characterized in that: and in the fifth step, 60 mu L of supernatant in the fourth step is taken, mixed, vortexed for 1-2min and then sample injection is carried out, and the steroid hormone is detected and analyzed by liquid chromatography-mass spectrometry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910443241.6A CN111983044B (en) | 2019-05-24 | 2019-05-24 | Detection method for analyzing steroid hormone based on double-derivative treatment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910443241.6A CN111983044B (en) | 2019-05-24 | 2019-05-24 | Detection method for analyzing steroid hormone based on double-derivative treatment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111983044A true CN111983044A (en) | 2020-11-24 |
| CN111983044B CN111983044B (en) | 2023-04-11 |
Family
ID=73437263
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910443241.6A Active CN111983044B (en) | 2019-05-24 | 2019-05-24 | Detection method for analyzing steroid hormone based on double-derivative treatment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111983044B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112763602A (en) * | 2020-12-24 | 2021-05-07 | 诸暨市中医医院 | Rapid detection method for steroid hormones in serum |
| CN114705787A (en) * | 2022-04-28 | 2022-07-05 | 天津国科医工科技发展有限公司 | Method for detecting 12 steroid hormones in dry blood spots based on derivatization |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050181514A1 (en) * | 2002-04-15 | 2005-08-18 | Xia Xu | Methods for separation and detection of ketosteroids and other carbonyl-containing compounds |
| CN103575827A (en) * | 2013-11-09 | 2014-02-12 | 中国海洋大学 | Method for detecting monosaccharide and preparation method for derivative reagent |
| CN103698414A (en) * | 2012-09-27 | 2014-04-02 | 中国科学院大连化学物理研究所 | Chemical derivatization based method for detection of steroid hormones in urine |
| CN103822998A (en) * | 2012-11-19 | 2014-05-28 | 中国科学院大连化学物理研究所 | Method for analyzing amine substances in dansyl chloride derived-plasma based on liquid chromatography mass spectrometry |
| CN105092753A (en) * | 2014-05-20 | 2015-11-25 | 中国科学院大连化学物理研究所 | Application of combination amine metabolism marker and kit and detection method thereof |
| CN105527350A (en) * | 2014-10-27 | 2016-04-27 | 中国科学院大连化学物理研究所 | Intracellular amino acid metabolic profiling analysis method |
| CN106191176A (en) * | 2015-05-06 | 2016-12-07 | 中国科学院大连化学物理研究所 | A kind of preparation method of resorufin glucuronide |
| CN106485082A (en) * | 2016-10-17 | 2017-03-08 | 南京医科大学 | A kind of method for building up of the OPLS DA diagnostic cast based on refining metabolism group and its application |
| CN108709941A (en) * | 2018-07-24 | 2018-10-26 | 曲阜师范大学 | A kind of determination method of the neurosteroid of hydroxyl |
| CN109374723A (en) * | 2018-09-30 | 2019-02-22 | 中国农业科学院油料作物研究所 | A kind of free fatty acid mass spectrometry quantitative analysis method based on double Derivatives |
| CN109709235A (en) * | 2019-02-25 | 2019-05-03 | 马红华 | Early diagnosis, prediction biomarker combinations, application and its measuring method of Alzheimer disease or slight old cognitive disorder |
-
2019
- 2019-05-24 CN CN201910443241.6A patent/CN111983044B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050181514A1 (en) * | 2002-04-15 | 2005-08-18 | Xia Xu | Methods for separation and detection of ketosteroids and other carbonyl-containing compounds |
| CN103698414A (en) * | 2012-09-27 | 2014-04-02 | 中国科学院大连化学物理研究所 | Chemical derivatization based method for detection of steroid hormones in urine |
| CN103822998A (en) * | 2012-11-19 | 2014-05-28 | 中国科学院大连化学物理研究所 | Method for analyzing amine substances in dansyl chloride derived-plasma based on liquid chromatography mass spectrometry |
| CN103575827A (en) * | 2013-11-09 | 2014-02-12 | 中国海洋大学 | Method for detecting monosaccharide and preparation method for derivative reagent |
| CN105092753A (en) * | 2014-05-20 | 2015-11-25 | 中国科学院大连化学物理研究所 | Application of combination amine metabolism marker and kit and detection method thereof |
| CN105527350A (en) * | 2014-10-27 | 2016-04-27 | 中国科学院大连化学物理研究所 | Intracellular amino acid metabolic profiling analysis method |
| CN106191176A (en) * | 2015-05-06 | 2016-12-07 | 中国科学院大连化学物理研究所 | A kind of preparation method of resorufin glucuronide |
| CN106485082A (en) * | 2016-10-17 | 2017-03-08 | 南京医科大学 | A kind of method for building up of the OPLS DA diagnostic cast based on refining metabolism group and its application |
| CN108709941A (en) * | 2018-07-24 | 2018-10-26 | 曲阜师范大学 | A kind of determination method of the neurosteroid of hydroxyl |
| CN109374723A (en) * | 2018-09-30 | 2019-02-22 | 中国农业科学院油料作物研究所 | A kind of free fatty acid mass spectrometry quantitative analysis method based on double Derivatives |
| CN109709235A (en) * | 2019-02-25 | 2019-05-03 | 马红华 | Early diagnosis, prediction biomarker combinations, application and its measuring method of Alzheimer disease or slight old cognitive disorder |
Non-Patent Citations (4)
| Title |
|---|
| JANA VITKU 等: "Development and validation of LC–MS/MS method for quantification of bisphenol A and estrogens in human plasma and seminal fluid", 《TALANTA》 * |
| LEONARDO DI DONNA 等: "Determination of ketosteroid hormones in meat by liquid chromatography tandem mass spectrometry and derivatization chemistry", 《ANAL BIOANAL CHEM》 * |
| 毋丹 等: "衍生化技术用于生物基质中性激素LC-MS检测的进展", 《药物分析杂志》 * |
| 胡秋菊 等: "衍生化技术用于生物基质中类固醇类激素分析的研究进展", 《医药导报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112763602A (en) * | 2020-12-24 | 2021-05-07 | 诸暨市中医医院 | Rapid detection method for steroid hormones in serum |
| CN114705787A (en) * | 2022-04-28 | 2022-07-05 | 天津国科医工科技发展有限公司 | Method for detecting 12 steroid hormones in dry blood spots based on derivatization |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111983044B (en) | 2023-04-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108663471B (en) | Method for determining contents of multiple endocrine disruptors in estuary sediments | |
| CN109633030A (en) | A kind of method that ultra performance liquid chromatography-QQ-TOF mass spectrometry detects amino acid in animal body fluid or tissue samples | |
| CN110702831B (en) | Kit for detecting serum testosterone hormone by ultra-high performance liquid chromatography-tandem mass spectrometry | |
| CN111983044B (en) | Detection method for analyzing steroid hormone based on double-derivative treatment | |
| CN114674961A (en) | Kit for synchronously detecting 17 steroid hormones in serum without derivatization and application thereof | |
| CN113049719A (en) | Method and kit for detecting free testosterone | |
| WO2020214811A1 (en) | Methods and systems for the detection of 11-oxo androgens by lc-ms/ms | |
| CN112964809A (en) | Kit for detecting multiple steroid hormones in biological body fluid and use method thereof | |
| CN111337610B (en) | Method for detecting trace estrogen, nonyl phenol and bisphenol A in complex environment matrix | |
| Lõhmus et al. | Determination of gestagens in kidney fat by liquid chromatography tandem mass spectrometry | |
| CN104597187A (en) | Method for rapidly and comprehensively detecting oligosaccharide on medicinal monoclonal antibody N-glycosylation site | |
| CN111766325A (en) | Sample pretreatment method for multiomic analysis and application thereof | |
| Śniegocki et al. | Analysis of β-agonists in different biological matrices by liquid chromatography–tandem mass spectrometry | |
| CN111579703A (en) | LC-MS/MS-based method for detecting and analyzing degradation products of bilirubin in biological sample | |
| CN112763602A (en) | Rapid detection method for steroid hormones in serum | |
| CN116338031A (en) | Method for detecting pollen sex hormone | |
| CN111257439A (en) | Method for detecting hydroxyl polybrominated diphenyl ethers in aquatic products by solid-phase extraction-ultra-high performance liquid chromatography tandem mass spectrometry | |
| CN106248825B (en) | Starting material A detection method in hydrochloride landiolol material medicine | |
| De Boer et al. | Mass spectrometric characterization of different norandrosterone derivatives by low‐cost mass spectrometric detectors using electron ionization and chemical ionization | |
| CN113671064B (en) | Detection method for quantitatively analyzing blood concentration of amlexanox in plasma | |
| CN103344726A (en) | Method for extraction of dicyandiamide component in dairy product | |
| CN111812243B (en) | Analysis method for reducing matrix effect in whole blood cyclosporine determination | |
| CN116990415A (en) | Non-targeted screening method for typical paralytic shellfish toxins in shellfish meat | |
| CN115963169B (en) | Detection method of carnitine and detection kit | |
| CN116642975A (en) | Mass spectrum detection method for six catecholamine hormones and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |