CN103823008A - Method for detecting unknown poison by establishing liquid chromatography-mass spectrometry database - Google Patents
Method for detecting unknown poison by establishing liquid chromatography-mass spectrometry database Download PDFInfo
- Publication number
- CN103823008A CN103823008A CN201410093316.XA CN201410093316A CN103823008A CN 103823008 A CN103823008 A CN 103823008A CN 201410093316 A CN201410093316 A CN 201410093316A CN 103823008 A CN103823008 A CN 103823008A
- Authority
- CN
- China
- Prior art keywords
- liquid chromatography
- sample
- mass
- database
- unknown
- 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
Abstract
The invention relates to a method for detecting unknown poison by establishing a liquid chromatography-mass spectrometry database, in particular to a method used for detecting unknown poison during food poisoning. According to the method, firstly, an ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry method is used for establishing a liquid chromatography-mass spectrometry database of common poison; then, a sample is subjected to supersonic extraction with methyl alcohol or acetonitrile, liquid chromatography-mass spectrometry data of an extracting solution are measured similarly and searched and compared in the liquid chromatogram-mass spectrometry database of common poison according to the retention time of the sample and mass spectrometry fragments, and the variety of the unknown poison in the sample is judged; and the unknown poisoning sample is simply extracted and directly measured and compared, and a screening result can be acquired in one hour, so that the detecting and treating time of the sample is greatly shortened, the detecting efficiency is improved, and technical support is provided for related events such as food poisoning and the like caused by unknown reasons.
Description
Technical field
The present invention relates to a kind of method that detects unknown poisonous substance, be specifically related to a kind of method that builds liquid chromatography-mass spectrography database and detect unknown poisonous substance, be used in particular for the detection of unknown poisonous substance in food poisoning.
Background technology
Poisonous substance refers under certain conditions, no matter in which way, low dose acts on body, produces physics or chemical action with body, and the destruction that causes body normal physiological function causes a series of pathological changes, the murderous material of threat to life even.Food poisoning refers to have been taken in the food that contains biological, chemical property poisonous and harmful substance or poisonous and harmful substance has been used as to food and takes the photograph noninfectious acute, the subacute disease occurring after people.According to statistics, the etesian food poisoning of China has hundreds of to thousands of, relates to number up to ten thousand.The healthy of serious harm people not only of poisoning by food, and cause bad social influence, cause extensive concern.Can be accurately, fast processing food poisoning become one of emphasis of the department technology such as health, public security capacity building.
Toxicological analysis in poisoning is different from general conventional analysis and separately has its feature, and as some toxicity symptom is difficult to and disease is distinguished, general Poisoning Cases mostly is unknown material analysis, if modern age poison type various to confirm as a certain just like look for a needle in a haystack; Experimental material is special, limited amount, can not regain, and analytical approach is changeable, sometimes needs to bear a legal liability etc.And, the identification and analysis General Requirements of poisonous substance is completed within the shortest time, just can not make according to a conventional method Analysis and Identification one by one.So toxicological analysis work must be determined check emphasis, there is target, carry out targetedly, to reach object accurately and rapidly.
In all food poisonings, poisoning 40% left and right that accounts for that chemical substance causes, the poisoning feature with morbidity urgency, toxicity symptom weight, fatal rate high (accounting for the over half of the lethal number of all food poisonings) of this class.When reply chemical food poisoming event, determine that fast and effectively intoxicating material is the key of subsequent treatment and clinical treatment.Investigating out in time poisoning reason, locking poisonous substance is to guarantee that doctor suits the remedy to the case, accurately processes the prerequisite of the condition of the injury, can promote like this Rehabilitation, significantly reduces the rate of being poisoned to death.So, in order to guarantee the accurate, timely of chemical food poisoming testing result, must centering poisons cross with poisonous substance source and do investigation and the sampling that dark people is careful, some are also set up in succession for the method for quick of predetermined substance (as nitrite, heavy metal class, arsenic, mercury, prussiate etc.).However, consider food poisoning diversity and complicacy, these fast detecting methods all have certain limitation and unicity, still have every year a large amount of poisonings can not find out its reason.Therefore, the examination confirmation work of unknown toxicity is still the huge challenge that sanitary inspection worker faces.
Present stage, the examination of unknown material is mainly to be compared with standard model and confirmed by mass spectrum.Along with the development of mass-spectrometric technique, inquire about to confirm that by the comparison of database unknown compound becomes relatively simple.Conventional organic mass spectrometry database is mainly the database mating with gas chromatography-mass spectrum technology at present, (more than 190000 plant compound to comprise the NIST mass spectral database of American National Standards Institute, more than 220000 spectrograms) and Wiley mass spectral database (more than 300000 plant compound, more than 400000 spectrograms), substantially contain common volatile poison.But for a lot of food poisonings that caused by the toxic compounds of difficulty volatilization, easily pyrolysis, existing commercialization mass spectrometric data storehouse far can not meet the needs of food poisoning emergency disposal.
For difficult volatile compound, current confirmation method generally adopts high performance liquid chromatography one quadrupole rod mass spectrum (LC-MS/MS), liquid chromatography one technology such as quadrupole rod/flight time mass spectrum (LC-Q-TOF) of connecting of connecting.But, because LC-MS generally adopts the mode of soft ionization, and the mass spectrum design concept difference of the liquid chromatography-mass spectrography of different company, analytical parameters is not quite similar, neither one is unified mass spectrogram comparable or coupling, the mass spectrogram difference that each company obtains may be very large, and this has brought difficulty just to the unification of the mass spectral database that adopts the analysis of liquid matter.But mass spectrogram quasi-molecular ion peak and ms fragment that the instrument of each company obtains are identical, can be used as rapid screening, contrast with the judged result of toxicity symptom, by liquid chromatography chromatographic column, mobile phase condition, retention time etc., can carry out further qualitative confirmation simultaneously.
The present invention, according to above-mentioned situation, builds the liquid chromatography mass database of common poisons, medicine, develops a kind of poisonous substance screening method based on liquid chromatography mass information, for the investigation of the events such as unknown cause food poisoning provides technology and method foundation.
Summary of the invention
The object of the present invention is to provide a kind of novel, can be by the method for the common poisons medicine of liquid chromatography mass information quick-searching and examination, according to existing data check, filter out the poisonous substance of common food poisoning, set up its LC-MS mass spectrometric data storehouse, this storehouse will be carried out qualitative based on retention time and ms fragment, can be used for the rapid screening of unknown intoxicating material, for the relevant accidents such as laboratory treatment food poisoning or drug poisoning provide technical support.
Structure liquid chromatography-mass spectrography database provided by the invention detects the method for unknown poisonous substance in sample, comprising: (1) adopts Ultra Performance Liquid Chromatography-level Four bar flight time mass spectrum method to build the liquid chromatography-mass spectrography database of common poisons; (2) sample preparation and detection, by methyl alcohol or the ultrasonic extract that extracts to obtain of acetonitrile for testing sample, by centrifugal described extract, get supernatant, under the method for testing and test condition identical with step (1), measure the liquid chromatography-mass spectrography figure of described supernatant; (3) the liquid chromatography-mass spectrography database of the common poisons described in liquid chromatography-mass spectrography figure step (2) Suo Shu and step (1) is compared, the kind of unknown poisonous substance in judgement sample.
The sample preparation of described step (2) is: the sample of 1.00g is put in 15mL tool plug centrifuge tube, and with 10mL methyl alcohol or the ultrasonic extraction of acetonitrile 10min, the centrifugal 5min of 10000rpm, produces supernatant, detects.
The comparison of described step (3) is that the liquid chromatography-mass spectrography database of retention time per sample and ms fragment and described common poisons carries out search comparison, the kind of unknown poisonous substance in judgement sample.
Described liquid chromatography-mass spectrography database comprises that more than 2000 plant the mass spectrogram of material, comprising saxitoxin (paralytic toxin, saxitoxin etc.), numb product (the heroin of poison, cocaine, methadone, triazolam, ketamine, haloperole etc.), mycotoxin (aflatoxin, patulin, chrysanthemum penicillin, fumonisins, ochratoxin, corn is eaten mould alcohols etc.), agricultural chemicals (pesticide, herbicide, germifuge, growth accelerator etc.), raticide (chloradion, bromine mouse ketone, Bromadiolone, Brodifacoum, flocoumafen, diphacinone, chlorophacinone etc.), hormone (estrogen, androgen, corticosteroid hormone, progestational hormone etc.), beta-receptor activator, receptor blocking agent, the drugs and toxicantses such as microbiotic, and register compound English name, No. CAS, molecular weight, molecular formula, acquisition condition, the information such as retention time.
The liquid chromatography-mass spectrography database concrete steps that described employing Ultra Performance Liquid Chromatography-level Four bar flight time mass spectrum method builds common poisons are as follows: 1.1 informations: collect the relevant information of common poisons medicine, comprise English name, No. CAS, molecular weight, molecular formula etc.; 1.2 standard solution preparations: weigh respectively more than 2000 and plant drugs and toxicants, take methyl alcohol as solvent, be mixed with the standard solution of 1-10mg/L; 1.3 data acquisitions: described standard solution is injected to Ultra Performance Liquid Chromatography instrument, again through the analysis of level Four bar-time of-flight mass spectrometer, wherein the chromatographic column of Ultra Performance Liquid Chromatography instrument is Waters BEH C18 (100mm × 2.1mm, m) chromatographic column of 1.7 μ, level Four bar-time of-flight mass spectrometer is chosen in respectively under positive ion mode, negative ion mode and carries out data acquisition, obtains the liquid chromatography mass figure of target drugs and toxicants; 1.4 spectrum storehouses build, and by target drugs and toxicants mass spectrogram, are added in liquid chromatography mass database, input the information such as English name, No. CAS, molecular weight, molecular formula, retention time simultaneously.
The instrument that Ultra Performance Liquid Chromatography-level Four bar flight time mass spectrum method adopts is: ACQUITY Ultra Performance Liquid Chromatography instrument and SYNAPT level Four bar time of-flight mass spectrometer (Q-TOF, Waters company of the U.S.)
Described chromatographic condition is: column temperature: 40 ℃; Mobile phase: A is acetonitrile mutually, and B is 0.1% (v/v) aqueous formic acid or water mutually, and when wherein mass spectrum adopts positive ion mode to gather, B is 0.1% (v/v) aqueous formic acid mutually, and when mass spectrum adopts negative ion mode to gather, B is water mutually; Flow velocity: 0.4mL/min; Eluent gradient elution program: 0～2min3%A; 2.0～14.0min3%A linearity rises to 100%A, keeps 1min, then gets back to initial flow and keeps mutually 2.5min, prepares sample introduction next time, sampling volume 5 μ l.
Described mass spectrum condition is: ion gun: electric spray ion source, positive ion mode (ESI+) and negative ion mode (ESI-); Ion source temperature: 110 ℃; Capillary voltage: 3.1kV; Desolventizing temperature degree: 400 ℃; Desolventizing airshed: 700L/h nitrogen; Taper hole voltage: 35V; Taper hole sweep gas: 50L/h: adopt MSE pattern, acquisition range: m/z50～1000Da; For several precision of ensuring the quality of products, carry out real time calibration with LEK (concentration 50ng/mL, m/z:556.2771).
The present invention is by liquid chromatography mass technology, set up liquid chromatography mass database and the application process thereof of common poisons, medicine, and more than 2000 Information in Mass Spectras of planting drugs and toxicants have been contained in this storehouse.For the material that difficulty is volatilized, polarity is stronger, do not need derivatization step, simple to operate.Unknown Poisoned Samples is directly measured comparison after simple extraction, can in 1 hour, obtain screening results (the wherein about 20min of sample pre-treatments, sample instrument about 20min detection time, about 10min of data retrieval time).Compared with traditional gaschromatographic mass spectrometric analysis, greatly shorten detection and the processing time of sample, improve detection efficiency, for the processing of the dependent events such as unknown cause food poisoning provides technical support.
Accompanying drawing explanation
Fig. 1 detects the method step figure of unknown poisonous substance in sample;
The chromatographic data figure that Fig. 2 A liquid chromatography mass storehouse builds;
The mass spectrometric data figure that Fig. 2 B liquid chromatography mass storehouse builds;
Chromatogram and the mass spectrogram of Shui An mountain, Fig. 3 Huairou Deep-fried eggplant starch isolation liquid, the wherein chromatogram of figure (A) for measuring under high collision energy condition, the mass spectrogram of figure (B) for measuring under high collision energy condition; The chromatogram of figure (C) for measuring under low collision energy condition, the mass spectrogram of figure (D) for measuring under low collision energy condition;
Chromatogram and the mass spectrogram of Fig. 4 clonidine standard items, the wherein chromatogram of figure (A) for measuring under high collision energy condition, the mass spectrogram of figure (B) for measuring under high collision energy condition; The chromatogram of figure (C) for measuring under low collision energy condition, the mass spectrogram of figure (D) for measuring under low collision energy condition;
Shui An mountain, Fig. 5 Huairou Deep-fried eggplant starch screening results mass spectrogram;
Chromatogram and the mass spectrogram of Fig. 6 Shandong Wenshang fried chicken sample extracting solution, the wherein chromatogram of figure (A) for measuring under high collision energy condition, the mass spectrogram of figure (B) for measuring under high collision energy condition; The chromatogram of figure (C) for measuring under low collision energy condition, the mass spectrogram of figure (D) for measuring under low collision energy condition;
Chromatogram and the mass spectrogram of Fig. 7 salinomycin standard items, the wherein chromatogram of figure (A) for measuring under high collision energy condition, the mass spectrogram of figure (B) for measuring under high collision energy condition; The chromatogram of figure (C) for measuring under low collision energy condition, the mass spectrogram of figure (D) for measuring under low collision energy condition;
Fig. 8 Shandong Wenshang fried chicken sample screening results mass spectrogram
Embodiment
Test analysis equipment, medicine and condition that present embodiment relates to are:
Instrument and equipment: ACQUITY Ultra Performance Liquid Chromatography instrument, SYNAPT level Four bar time of-flight mass spectrometer (Q-TOF, Waters company of the U.S.), ultrasonic washing instrument (KH1 type, Kunshan He Chuan ultrasonic instrument company limited), hydro-extractor (X-22R, Beckman company of the U.S.).
Reagent: methyl alcohol, acetonitrile, the drugs and toxicants standard substance of look general level.
The chromatographic condition of Ultra Performance Liquid Chromatography instrument:
Sampling volume: 5 μ l;
Chromatographic column: (100mm × 2.1mm, 1.7 μ m) for Waters BEH C18
Column temperature: 40 ℃;
Mobile phase: A is acetonitrile mutually, and B is 0.1% (v/v) aqueous formic acid or water mutually, and when wherein mass spectrum adopts positive ion mode to gather, B is 0.1% (v/v) aqueous formic acid mutually, and when mass spectrum adopts negative ion mode to gather, B is water mutually;
Flow velocity: 0.4mL/min;
Eluent gradient elution program: 0～2min3%A; 2.0～14.0min3%A linearity rises to 100%A, keeps 1min, then gets back to initial flow and keeps mutually 2.5min, prepares sample introduction next time.
The mass spectrum condition of level Four bar time of-flight mass spectrometer:
Ion gun: electric spray ion source;
Positive ion mode (ESI+) and negative ion mode (ESI-);
Ion source temperature: 110 ℃;
Capillary voltage: 3.1kV;
Desolventizing temperature degree: 400 ℃;
Desolventizing airshed: 700L/h nitrogen;
Taper hole voltage: 35V;
Taper hole sweep gas: 50L/h;
Adopt MSE pattern, acquisition range: m/z50～1000Da; For several precision of ensuring the quality of products, carry out real time calibration with LEK (concentration 50ng/mL, m/z:556.2771).
As shown in Figure 1, structure liquid chromatography-mass spectrography database of the present invention detects the method for unknown poisonous substance in sample, comprise: (1) adopts Ultra Performance Liquid Chromatography-level Four bar flight time mass spectrum method to build the liquid chromatography-mass spectrography database of common poisons, liquid chromatography-mass spectrography database comprises that more than 2000 plant the mass spectrogram of material, comprising saxitoxin (paralytic toxin, saxitoxin etc.), numb product (the heroin of poison, cocaine, methadone, triazolam, ketamine, haloperole etc.), mycotoxin (aflatoxin, patulin, chrysanthemum penicillin, fumonisins, ochratoxin, corn is eaten mould alcohols etc.), agricultural chemicals (pesticide, herbicide, germifuge, growth accelerator etc.), raticide (chloradion, bromine mouse ketone, Bromadiolone, Brodifacoum, flocoumafen, diphacinone, chlorophacinone etc.), hormone (estrogen, androgen, corticosteroid hormone, progestational hormone etc.), beta-receptor activator, receptor blocking agent, the drugs and toxicantses such as microbiotic, and registered compound English name, No. CAS, molecular weight, molecular formula, acquisition condition, the information such as retention time, (2) sample preparation and detection, the sample of 1.00g is put in 15mL tool plug centrifuge tube, with 10mL methyl alcohol or the ultrasonic extraction of acetonitrile 10min, the centrifugal 5min of 10000rpm, produce supernatant, under the method for testing and test condition identical with step (1), measure the liquid chromatography-mass spectrography figure of described supernatant, (3) the liquid chromatography-mass spectrography database of the common poisons described in liquid chromatography-mass spectrography figure step (2) Suo Shu and step (1) is compared, the kind of unknown poisonous substance in judgement sample.
The liquid chromatography-mass spectrography database concrete steps that described structure Ultra Performance Liquid Chromatography-level Four bar flight time mass spectrum method builds common poisons are as follows: 1. information: collect the relevant information of common poisons medicine, comprise English name, No. CAS, molecular weight, molecular formula etc.; 2. standard solution preparation: weigh respectively more than 2000 and plant drugs and toxicants, take methyl alcohol as solvent, be mixed with the standard solution of 1-10mg/L; 3. data acquisition: described standard solution is injected to Ultra Performance Liquid Chromatography instrument, again through the analysis of level Four bar-time of-flight mass spectrometer, wherein the chromatographic column of Ultra Performance Liquid Chromatography instrument is Waters BEH C18 (100mm × 2.1mm, m) chromatographic column of 1.7 μ, level Four bar-time of-flight mass spectrometer is chosen in respectively under positive ion mode, negative ion mode and carries out data acquisition, obtains the liquid chromatography mass figure of target drugs and toxicants; 4. spectrum storehouse builds, and by target drugs and toxicants mass spectrogram, is added in liquid chromatography mass database, inputs the information such as English name, No. CAS, molecular weight, molecular formula, retention time simultaneously.
The collection of standard drugs and toxicants liquid chromatography mass diagram data comprises in addition: the liquid chromatography mass figure gathering under high collision energy and low collision energy, as shown in Figure 2 A and 2B, determines retention time and Information in Mass Spectra;
Target drugs and toxicants mass spectrogram is added into liquid chromatography mass database to be comprised: in mass spectrogram window, click successively [Edit], [Library], [Append ... ] carry out self-built mass spectral database operation; Editor's mass spectrogram relevant information, input English name, No. CAS, molecular formula, molecular weight, retention time, ion drainage pattern and collision energy;
Two mass spectrogram information that comprise every kind of compound in final self-built mass spectral database, its corresponding collision energy is different; Every kind of medicine comprises two two-dimentional spectrograms, both can effectively improve retrieval rate, reduces again the output quantity of automatic result for retrieval.
The database building during for the examination of unknown material, must guarantee feasibility, accuracy and the reliability of each examination parameter.When examination, mainly adopt ChromaLynxTM software to analyze, can use individually or simultaneously two databases that establish to carry out data match analysis, utilize mass spectrum deconvolution techniques by with database in spectrogram and the accurately correlation parameter contrast such as molion mass number, fragmention mass number and automatically identify the candidate substances at each peak; While using two databases to carry out examination simultaneously, relate to the optimization of discrimination method (Identify method) and spectrum library searching method (Library search method), wherein, discrimination method editor's is the correlation parameter that adopts text database, and spectrum library searching method is the correlation parameter of spectrum library.
The improper meeting that arranges of discrimination method parameter, library searching parameter causes the inaccurate of Search Results, therefore, must first optimize the correlation parameter of two methods while carrying out data examination.The optimization of discrimination method: retention time deviation window, determine according to retention time deviation in material retention time and database in actual sample; High-quality is counted the characteristic that precision is high resolution mass spectrum, and mass number deviation window is the important parameter of several precision of ensuring the quality of products, and the difference of two mass numbers of General Requirements is less than or equal to 3mDa.The optimization of spectrum library searching method: set appropriate coupling factor, comprise the setting of higher limit and lower limit, all set according to the disturbed condition of actual sample mesostroma, in the time that interference is larger, two parameters are reduced accordingly, otherwise increase by two parameter values; Select retention time as one of them examination factor, and set deviation window.The screening method of final optimization pass is for the examination of actual sample.Embodiment in April, 12010 Huairou Shui An mountain Poisoned Samples examination
Noon on April 23rd, 2010, probably there is more than 200 visitor at Shui An mountain, Huairou, Beijing dining in restaurant, the first patient is with after the meal less than occurring toxicity symptom half an hour, end 1 o'clock on the 24th April, there is symptom (blood pressure is low, heart rate delays, feel run-down, muscle is numb, blurred vision, and myosis, n and V, pale complexion etc. appear in some patients were) in various degree in existing 100 people.
The vegetable that gathers ill personnel detects, and takes 1g food samples in 50mL centrifuge tube, adds 10mL methyl alcohol whirlpool to mix, ultrasonic extraction 10min.Centrifugal rear supernatant proceeds to and in 2ml sample injection bottle, gathers its liquid chromatography mass information, carry out search comparison with built common poisons medicine liquid chromatography-mass spectrography database, 22 food samples have been carried out respectively to examination, getting rid of 12 negative sample (salt, soy sauce, oil, water-starch etc.) afterwards, in the dried starch of using at Deep-fried eggplant, detect clonidine, its chromatogram and mass spectrogram are as shown in Figure 3, the retention time (3.78min) of target compound is all consistent with the clonidine standard items of Fig. 4 with feature ms fragment (m/z230.023), mass spectral database screening results is as Fig. 5.This time for sample pretreatment is 10min, detection time 15min, comparison time is 5min, whole examination process 30min consuming time.
The Wenshang Poisoned Samples examination of embodiment Shandong in February, 22008
On February 4th, 2008, after Kang Yi town, Wenshang County, Shandong Province Hu Zhuan village one family villager's family party, there is dim eyesight in 18 people, limbs pain, numbness and dyskinesia (obvious with two lower limb), companion's nausea and vomiting, without symptoms such as stomachache, diarrhoea and heatings, weight differs.The 5 parts of food samples (fried chicken, fried fish tartar souce etc.) that use of having a dinner party are detected, take about 2g food samples in 50mL centrifuge tube, add 10mL methyl alcohol whirlpool to mix, ultrasonic extraction 10min.Centrifugal rear supernatant proceeds to and in 2ml sample injection bottle, gathers its liquid chromatography mass information, carry out search comparison with built common poisons medicine liquid chromatography-mass spectrography database, in 4 duplicate samples such as fried chicken, finding salinomycin, Fig. 6 has provided the chromatogram of fried chicken sample and the mass spectrogram of drug target, its retention time and characteristic ion and salinomycin standard items (Fig. 7) coincide good, and mass spectral database screening results is as Fig. 8.This time for sample pretreatment is 12min, detection time 15min, comparison time is 5min, whole examination process 32min consuming time.
The present invention, for the material that difficulty is volatilized, polarity is stronger, does not need derivatization step, and simple to operate, the pre-treatment time is short, detects fast, and detection efficiency is high, for the processing of the dependent events such as unknown cause food poisoning provides technical support.
The explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
Claims (8)
1. the method that builds unknown poisonous substance in liquid chromatography-mass spectrography database detection sample, is characterized in that, comprising: (1) adopts Ultra Performance Liquid Chromatography-level Four bar flight time mass spectrum method to build the liquid chromatography-mass spectrography database of common poisons; (2) sample preparation and detection, by methyl alcohol or the ultrasonic extract that extracts to obtain of acetonitrile for testing sample, by centrifugal described extract, get supernatant, under the method for testing and test condition identical with step (1), measure the liquid chromatography-mass spectrography figure of described supernatant; (3) the liquid chromatography-mass spectrography database of the common poisons described in liquid chromatography-mass spectrography figure step (2) Suo Shu and step (1) is compared, the kind of unknown poisonous substance in judgement sample.
2. structure liquid chromatography-mass spectrography database according to claim 1 detects the method for unknown poisonous substance in sample, it is characterized in that, the step that described step (1) adopts Ultra Performance Liquid Chromatography-flight time mass spectrum method to build the liquid chromatography-mass spectrography database of common poisons comprises: 1.1 informations, collect the relevant information of common poisons medicine, comprise English name, No. CAS, molecular weight, molecular formula etc.; 1.2 standard solution preparations, weigh respectively more than 2000 and plant drugs and toxicants, take methyl alcohol as solvent, are mixed with the standard solution of 1-10mg/L; 1.3 data acquisition, described standard solution is injected to Ultra Performance Liquid Chromatography instrument, again through the analysis of level Four bar-time of-flight mass spectrometer, wherein the chromatographic column of Ultra Performance Liquid Chromatography instrument is Waters BEH C18 (100mm × 2.1mm, m) chromatographic column of 1.7 μ, level Four bar-time of-flight mass spectrometer is chosen in respectively under positive ion mode, negative ion mode and carries out data acquisition, obtains the liquid chromatography mass figure of target drugs and toxicants; 1.4 spectrum storehouses build, and by target drugs and toxicants mass spectrogram, are added in liquid chromatography mass database, input the information such as English name, No. CAS, molecular weight, molecular formula, retention time simultaneously.
3. structure liquid chromatography-mass spectrography database according to claim 2 detects the method for unknown poisonous substance in sample, it is characterized in that, the chromatographic condition of described step 1.3 is: column temperature: 40 ℃; Mobile phase: A is acetonitrile mutually, and B is 0.1% (v/v) aqueous formic acid or water mutually, and when wherein mass spectrum adopts positive ion mode to gather, B is 0.1% (v/v) aqueous formic acid mutually, and when mass spectrum adopts negative ion mode to gather, B is water mutually; Flow velocity: 0.4mL/min, eluent gradient elution program: 0～2min3%A; 2.0～14.0min3%A linearity rises to 100%A, keeps 1min, then gets back to initial flow and keeps mutually 2.5min, prepares sample introduction next time, sampling volume 5 μ l; Mass spectrum condition: ion gun: electric spray ion source, positive ion mode (ESI+) and negative ion mode (ESI-); Ion source temperature: 110 ℃; Capillary voltage: 3.1kV; Desolventizing temperature degree: 400 ℃; Desolventizing airshed: 700L/h nitrogen; Taper hole voltage: 35V; Taper hole sweep gas: 50L/h; Adopt MSE pattern, acquisition range: m/z50～1000Da; Carry out real time calibration with LEK (concentration 50ng/mL, m/z:556.2771).
4. structure liquid chromatography-mass spectrography database according to claim 1 detects the method for unknown poisonous substance in sample, it is characterized in that, the sample preparation of described step (2) is: the sample of 1.00g is put in 15mL tool plug centrifuge tube, with 10mL methyl alcohol or the ultrasonic extraction of acetonitrile 10min, the centrifugal 5min of 10000rpm, produces supernatant.
5. structure liquid chromatography-mass spectrography database according to claim 1 detects the method for unknown poisonous substance in sample, it is characterized in that, the comparison of described step (3) is that the liquid chromatography-mass spectrography database of retention time per sample and ms fragment and described common poisons carries out search comparison, the kind of unknown poisonous substance in judgement sample.
6. detect the method for unknown poisonous substance in sample according to the arbitrary described structure liquid chromatography-mass spectrography database of claim 1 to 5, it is characterized in that, unknown poisonous substance comprises the drugs and toxicantses such as saxitoxin, malicious numb product, mycotoxin, agricultural chemicals, raticide, hormone, beta-receptor activator, receptor blocking agent, microbiotic.
7. structure liquid chromatography-mass spectrography database according to claim 6 detects the method for unknown poisonous substance in sample, it is characterized in that, described saxitoxin comprises paralytic toxin, saxitoxin etc.; The numb product of described poison comprise heroin, cocaine, methadone, triazolam, ketamine, haloperole etc.; Mycotoxin comprises that aflatoxin, patulin, chrysanthemum penicillin, fumonisins, ochratoxin, corn eat mould alcohols etc.; Agricultural chemicals comprises Insecticides (tech) & Herbicides (tech), germifuge, growth accelerator etc.; Raticide comprises chloradion, bromine mouse ketone, Bromadiolone, Brodifacoum, flocoumafen, diphacinone, chlorophacinone etc.; Hormone comprises estrogen, androgen, corticosteroid hormone, progestational hormone etc.
8. structure liquid chromatography-mass spectrography database according to claim 6 detects the method for unknown poisonous substance in sample, it is characterized in that, can be used for food poisoning analysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410093316.XA CN103823008B (en) | 2014-03-14 | 2014-03-14 | Build the method that liquid chromatography-mass spectrography database detects unknown poisonous substance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410093316.XA CN103823008B (en) | 2014-03-14 | 2014-03-14 | Build the method that liquid chromatography-mass spectrography database detects unknown poisonous substance |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103823008A true CN103823008A (en) | 2014-05-28 |
| CN103823008B CN103823008B (en) | 2016-03-02 |
Family
ID=50758171
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410093316.XA Active CN103823008B (en) | 2014-03-14 | 2014-03-14 | Build the method that liquid chromatography-mass spectrography database detects unknown poisonous substance |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103823008B (en) |
Cited By (43)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104360001A (en) * | 2014-11-26 | 2015-02-18 | 公安部禁毒情报技术中心 | Discriminating method for heroin origins |
| CN104458987A (en) * | 2014-11-26 | 2015-03-25 | 公安部禁毒情报技术中心 | Method for detecting 25 neutral or acidic impurities in heroin |
| CN104515821A (en) * | 2014-11-25 | 2015-04-15 | 山东省农业科学院农业质量标准与检测技术研究所 | Corn kernel kumonisins rapid determination method |
| CN104764843A (en) * | 2015-02-27 | 2015-07-08 | 潍坊出入境检验检疫局综合技术服务中心 | Method for detection of electronegative element containing pesticides by negative chemical ionization mass spectrum database |
| CN105301147A (en) * | 2014-06-17 | 2016-02-03 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for detecting diethylstilbestrol hormones in liquid milk according to liquid chromatography-mass spectrometer method |
| CN105467057A (en) * | 2015-12-28 | 2016-04-06 | 中国检验检疫科学研究院 | GC-Q-TOF/MS detection technology for 708 pesticide residues in citrus fruits |
| CN105467056A (en) * | 2015-12-28 | 2016-04-06 | 中国检验检疫科学研究院 | GC-Q-TOF(gas chromatography-quadrupole-time of flight)/MS(mass spectrography) detecting technology for 708 pesticide residues in solanaceous vegetables |
| CN105510499A (en) * | 2015-12-28 | 2016-04-20 | 中国检验检疫科学研究院 | GC-Q-TOF/MS detection technology of 708 pesticide residues in melon vegetables |
| CN105588911A (en) * | 2015-12-28 | 2016-05-18 | 中国检验检疫科学研究院 | GC-Q-TOF/MS detection technology for 708 pesticide residues in bud vegetables |
| CN105651920A (en) * | 2015-12-28 | 2016-06-08 | 中国检验检疫科学研究院 | GC-Q-TOF/MS (Gas Chromatography-Quadrupole-Time-Of-Flight/Mass Spectrometry) detection technology for 708 pesticide residues in bulb vegetables |
| CN105651919A (en) * | 2015-12-28 | 2016-06-08 | 中国检验检疫科学研究院 | GC-Q-TOF/MS detection technology for detecting 708 kinds of pesticide residues in brassica vegetables |
| CN105675701A (en) * | 2015-12-28 | 2016-06-15 | 中国检验检疫科学研究院 | GC-Q-TOF/MS detection technology of 708 pesticide residues in legume vegetables |
| CN105675702A (en) * | 2015-12-28 | 2016-06-15 | 中国检验检疫科学研究院 | GC-Q-TOF/MS detection technology of 708 pesticide residues in edible mushrooms |
| CN105675703A (en) * | 2015-12-28 | 2016-06-15 | 中国检验检疫科学研究院 | LC-Q-TOF/MS detection technology for 544 pesticide residues in edible mushrooms |
| CN105738460A (en) * | 2015-12-28 | 2016-07-06 | 中国检验检疫科学研究院 | LC-Q-TOF/MS detection technology for 544 pesticide residues in leaf vegetables |
| CN105823832A (en) * | 2015-12-28 | 2016-08-03 | 中国检验检疫科学研究院 | LC-Q-TOF/MS detection technology for 544 pesticide residues in kernel fruit |
| CN106370747A (en) * | 2016-08-26 | 2017-02-01 | 晨光生物科技集团股份有限公司 | Method for detecting ochratoxin A in capsicum extract |
| CN106404474A (en) * | 2015-12-25 | 2017-02-15 | 首都医科大学附属北京同仁医院 | Extraction process for filamentous fungus protein used for mass spectrum identification |
| CN106442772A (en) * | 2016-09-05 | 2017-02-22 | 司法部司法鉴定科学技术研究所 | Method for detecting and analyzing anticoagulant rodenticides in blood |
| CN106770721A (en) * | 2016-11-29 | 2017-05-31 | 百奥森（江苏）食品安全科技有限公司 | A kind of method for quick of patulin |
| CN106950327A (en) * | 2017-03-13 | 2017-07-14 | 中国水产科学研究院黄海水产研究所 | The examination of saxitoxin and confirmation method in complex matrices |
| CN107478757A (en) * | 2017-05-08 | 2017-12-15 | 公安部物证鉴定中心 | Method for preparing purified for the ketamine standard substance of forensic science illicit drugs inspection |
| CN107478747A (en) * | 2017-05-10 | 2017-12-15 | 山东省公安厅 | The liquid chromatography mass screening method of unknown poisonous substance in blood |
| CN107543891A (en) * | 2017-03-29 | 2018-01-05 | 中国检验检疫科学研究院 | The screening method of androgen chemical risk material in a kind of washing product |
| CN108303486A (en) * | 2017-12-05 | 2018-07-20 | 广东出入境检验检疫局检验检疫技术中心 | The non-targeted object rapid detection method of forbidden drug in a kind of health food |
| CN108445099A (en) * | 2018-03-12 | 2018-08-24 | 中国检验检疫科学研究院 | The assay method of 12 kinds of local anesthetics in a kind of cosmetics |
| CN108490098A (en) * | 2018-05-21 | 2018-09-04 | 安徽瑞思威尔科技有限公司 | The non-targeted quick screening method of unknown pesticide residue in a kind of white wine |
| CN108956801A (en) * | 2018-05-21 | 2018-12-07 | 安徽瑞思威尔科技有限公司 | The non-targeted quick screening method of unknown mycotoxin in a kind of white wine |
| CN109239247A (en) * | 2018-11-20 | 2019-01-18 | 西安交通大学 | A kind of liquid chromatogram is without reference substance method for qualitative analysis |
| CN109557197A (en) * | 2017-04-17 | 2019-04-02 | 中国检验检疫科学研究院 | Agricultural chemical compound electronic identity database and detection method in edible agricultural product based on GC-Q-Orbitrap |
| CN109613126A (en) * | 2018-11-01 | 2019-04-12 | 中国环境科学研究院 | The measuring method of illicit drug and its metabolite in a kind of fish body |
| CN109932467A (en) * | 2018-08-10 | 2019-06-25 | 烟台出入境检验检疫局检验检疫技术中心 | Ultra performance liquid chromatography-level four bars/high resolution mass spectrometry measurement Aflatoxin in Peanut byHigh and pesticide residue method |
| CN110110743A (en) * | 2019-03-26 | 2019-08-09 | 中国检验检疫科学研究院 | A kind of seven class mass spectrogram automatic recognition system of world's common pesticides and chemical pollutant and method based on cloud platform |
| CN111220754A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院大连化学物理研究所 | Ginseng recognition platform and ginseng recognition method using same |
| CN111220751A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院大连化学物理研究所 | Pseudo-ginseng identification platform and pseudo-ginseng identification method using same |
| CN111220753A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院大连化学物理研究所 | Sophora flavescens recognition platform and sophora flavescens recognition method using same |
| CN111220752A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院大连化学物理研究所 | American ginseng identification platform and American ginseng identification method using same |
| CN111222524A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院大连化学物理研究所 | Albizzia julibrissin identification platform and albizzia julibrissin identification method using same |
| CN113340873A (en) * | 2021-08-09 | 2021-09-03 | 北京市疾病预防控制中心 | SERS system for simultaneously detecting multiple toxic substances |
| CN113671070A (en) * | 2021-07-30 | 2021-11-19 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | Establishment and application of high-throughput screening mass spectrum database for cosmetic safety risk substances |
| CN114047280A (en) * | 2021-10-21 | 2022-02-15 | 苏州药明康德新药开发有限公司 | Method for detecting content of non-volatile unknown substances in medical instrument leaching liquor |
| CN115015403A (en) * | 2022-04-08 | 2022-09-06 | 浙江大学 | Rapid, comprehensive and stable identification method for unknown poison |
| CN115248271A (en) * | 2022-06-07 | 2022-10-28 | 浙江理工大学绍兴生物医药研究院有限公司 | Qualitative analysis method for volatile components of salvia officinalis |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040013740A1 (en) * | 2000-05-17 | 2004-01-22 | Dirk Weickmann | Dendritic cell loaded with toxic substances |
| US20100197521A1 (en) * | 2007-07-24 | 2010-08-05 | The Trustees Of Princeton University | Organo-cascade catalysis: one-pot production of chemical libraries |
| CN101859305A (en) * | 2009-04-13 | 2010-10-13 | 北京市疾病预防控制中心 | Liquid chromatogram and mass spectrum database of common poisons and medicines |
| CN102338789A (en) * | 2011-04-22 | 2012-02-01 | 上海谱尼测试技术有限公司 | Fast instrumental analysis method for aflatoxins in foods |
-
2014
- 2014-03-14 CN CN201410093316.XA patent/CN103823008B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040013740A1 (en) * | 2000-05-17 | 2004-01-22 | Dirk Weickmann | Dendritic cell loaded with toxic substances |
| US20100197521A1 (en) * | 2007-07-24 | 2010-08-05 | The Trustees Of Princeton University | Organo-cascade catalysis: one-pot production of chemical libraries |
| CN101859305A (en) * | 2009-04-13 | 2010-10-13 | 北京市疾病预防控制中心 | Liquid chromatogram and mass spectrum database of common poisons and medicines |
| CN102338789A (en) * | 2011-04-22 | 2012-02-01 | 上海谱尼测试技术有限公司 | Fast instrumental analysis method for aflatoxins in foods |
Non-Patent Citations (1)
| Title |
|---|
| 高馥蝶等: "超高效液相色谱-四级杆-飞行时间质谱法快速筛查牛奶中的农药和兽药残留", 《色谱》 * |
Cited By (55)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105301147A (en) * | 2014-06-17 | 2016-02-03 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for detecting diethylstilbestrol hormones in liquid milk according to liquid chromatography-mass spectrometer method |
| CN104515821A (en) * | 2014-11-25 | 2015-04-15 | 山东省农业科学院农业质量标准与检测技术研究所 | Corn kernel kumonisins rapid determination method |
| CN104515821B (en) * | 2014-11-25 | 2015-12-30 | 山东省农业科学院农业质量标准与检测技术研究所 | The rapid assay methods of fumonisin in a kind of corn kernel |
| CN104458987A (en) * | 2014-11-26 | 2015-03-25 | 公安部禁毒情报技术中心 | Method for detecting 25 neutral or acidic impurities in heroin |
| CN104360001A (en) * | 2014-11-26 | 2015-02-18 | 公安部禁毒情报技术中心 | Discriminating method for heroin origins |
| CN104360001B (en) * | 2014-11-26 | 2017-02-22 | 公安部禁毒情报技术中心 | Discriminating method for heroin origins |
| CN104458987B (en) * | 2014-11-26 | 2016-04-13 | 公安部禁毒情报技术中心 | 25 kinds of neutrality in heroin or the detection method of acid impurities |
| CN104764843A (en) * | 2015-02-27 | 2015-07-08 | 潍坊出入境检验检疫局综合技术服务中心 | Method for detection of electronegative element containing pesticides by negative chemical ionization mass spectrum database |
| CN106404474A (en) * | 2015-12-25 | 2017-02-15 | 首都医科大学附属北京同仁医院 | Extraction process for filamentous fungus protein used for mass spectrum identification |
| CN105675702A (en) * | 2015-12-28 | 2016-06-15 | 中国检验检疫科学研究院 | GC-Q-TOF/MS detection technology of 708 pesticide residues in edible mushrooms |
| CN105467056A (en) * | 2015-12-28 | 2016-04-06 | 中国检验检疫科学研究院 | GC-Q-TOF(gas chromatography-quadrupole-time of flight)/MS(mass spectrography) detecting technology for 708 pesticide residues in solanaceous vegetables |
| CN105651920A (en) * | 2015-12-28 | 2016-06-08 | 中国检验检疫科学研究院 | GC-Q-TOF/MS (Gas Chromatography-Quadrupole-Time-Of-Flight/Mass Spectrometry) detection technology for 708 pesticide residues in bulb vegetables |
| CN105651919A (en) * | 2015-12-28 | 2016-06-08 | 中国检验检疫科学研究院 | GC-Q-TOF/MS detection technology for detecting 708 kinds of pesticide residues in brassica vegetables |
| CN105675701A (en) * | 2015-12-28 | 2016-06-15 | 中国检验检疫科学研究院 | GC-Q-TOF/MS detection technology of 708 pesticide residues in legume vegetables |
| CN105467057A (en) * | 2015-12-28 | 2016-04-06 | 中国检验检疫科学研究院 | GC-Q-TOF/MS detection technology for 708 pesticide residues in citrus fruits |
| CN105675703A (en) * | 2015-12-28 | 2016-06-15 | 中国检验检疫科学研究院 | LC-Q-TOF/MS detection technology for 544 pesticide residues in edible mushrooms |
| CN105738460A (en) * | 2015-12-28 | 2016-07-06 | 中国检验检疫科学研究院 | LC-Q-TOF/MS detection technology for 544 pesticide residues in leaf vegetables |
| CN105823832A (en) * | 2015-12-28 | 2016-08-03 | 中国检验检疫科学研究院 | LC-Q-TOF/MS detection technology for 544 pesticide residues in kernel fruit |
| CN105588911A (en) * | 2015-12-28 | 2016-05-18 | 中国检验检疫科学研究院 | GC-Q-TOF/MS detection technology for 708 pesticide residues in bud vegetables |
| CN105510499A (en) * | 2015-12-28 | 2016-04-20 | 中国检验检疫科学研究院 | GC-Q-TOF/MS detection technology of 708 pesticide residues in melon vegetables |
| CN106370747A (en) * | 2016-08-26 | 2017-02-01 | 晨光生物科技集团股份有限公司 | Method for detecting ochratoxin A in capsicum extract |
| CN106370747B (en) * | 2016-08-26 | 2019-03-19 | 晨光生物科技集团股份有限公司 | The detection method of ochratoxin A in pepper extract |
| CN106442772A (en) * | 2016-09-05 | 2017-02-22 | 司法部司法鉴定科学技术研究所 | Method for detecting and analyzing anticoagulant rodenticides in blood |
| CN106770721A (en) * | 2016-11-29 | 2017-05-31 | 百奥森（江苏）食品安全科技有限公司 | A kind of method for quick of patulin |
| CN106950327A (en) * | 2017-03-13 | 2017-07-14 | 中国水产科学研究院黄海水产研究所 | The examination of saxitoxin and confirmation method in complex matrices |
| CN107543891A (en) * | 2017-03-29 | 2018-01-05 | 中国检验检疫科学研究院 | The screening method of androgen chemical risk material in a kind of washing product |
| CN107543891B (en) * | 2017-03-29 | 2020-01-03 | 中国检验检疫科学研究院 | Screening method for androgen chemical risk substances in washing and caring products |
| CN109557197B (en) * | 2017-04-17 | 2019-10-18 | 中国检验检疫科学研究院 | The method for building up and detection method of agricultural chemical compound electronic identity database in edible agricultural product based on GC-Q-Orbitrap |
| CN109557197A (en) * | 2017-04-17 | 2019-04-02 | 中国检验检疫科学研究院 | Agricultural chemical compound electronic identity database and detection method in edible agricultural product based on GC-Q-Orbitrap |
| CN107478757A (en) * | 2017-05-08 | 2017-12-15 | 公安部物证鉴定中心 | Method for preparing purified for the ketamine standard substance of forensic science illicit drugs inspection |
| CN107478757B (en) * | 2017-05-08 | 2019-12-06 | 公安部物证鉴定中心 | Method for purifying and preparing ketamine standard substance for forensic science drug detection |
| CN107478747A (en) * | 2017-05-10 | 2017-12-15 | 山东省公安厅 | The liquid chromatography mass screening method of unknown poisonous substance in blood |
| CN107478747B (en) * | 2017-05-10 | 2019-11-08 | 山东省公安厅 | The liquid chromatography-mass spectrography screening method of unknown poisonous substance in blood |
| CN108303486A (en) * | 2017-12-05 | 2018-07-20 | 广东出入境检验检疫局检验检疫技术中心 | The non-targeted object rapid detection method of forbidden drug in a kind of health food |
| CN108445099A (en) * | 2018-03-12 | 2018-08-24 | 中国检验检疫科学研究院 | The assay method of 12 kinds of local anesthetics in a kind of cosmetics |
| CN108445099B (en) * | 2018-03-12 | 2020-12-29 | 中国检验检疫科学研究院 | Method for measuring 12 local anesthetics in cosmetics |
| CN108956801A (en) * | 2018-05-21 | 2018-12-07 | 安徽瑞思威尔科技有限公司 | The non-targeted quick screening method of unknown mycotoxin in a kind of white wine |
| CN108490098A (en) * | 2018-05-21 | 2018-09-04 | 安徽瑞思威尔科技有限公司 | The non-targeted quick screening method of unknown pesticide residue in a kind of white wine |
| CN109932467A (en) * | 2018-08-10 | 2019-06-25 | 烟台出入境检验检疫局检验检疫技术中心 | Ultra performance liquid chromatography-level four bars/high resolution mass spectrometry measurement Aflatoxin in Peanut byHigh and pesticide residue method |
| CN109613126B (en) * | 2018-11-01 | 2020-11-03 | 中国环境科学研究院 | Method for determining illegal drugs and metabolites thereof in fish body |
| CN109613126A (en) * | 2018-11-01 | 2019-04-12 | 中国环境科学研究院 | The measuring method of illicit drug and its metabolite in a kind of fish body |
| CN109239247A (en) * | 2018-11-20 | 2019-01-18 | 西安交通大学 | A kind of liquid chromatogram is without reference substance method for qualitative analysis |
| CN111222524A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院大连化学物理研究所 | Albizzia julibrissin identification platform and albizzia julibrissin identification method using same |
| CN111220751A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院大连化学物理研究所 | Pseudo-ginseng identification platform and pseudo-ginseng identification method using same |
| CN111220753A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院大连化学物理研究所 | Sophora flavescens recognition platform and sophora flavescens recognition method using same |
| CN111220752A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院大连化学物理研究所 | American ginseng identification platform and American ginseng identification method using same |
| CN111220754A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院大连化学物理研究所 | Ginseng recognition platform and ginseng recognition method using same |
| CN110110743B (en) * | 2019-03-26 | 2019-12-31 | 中国检验检疫科学研究院 | Automatic recognition system and method for seven-class mass spectrum |
| CN110110743A (en) * | 2019-03-26 | 2019-08-09 | 中国检验检疫科学研究院 | A kind of seven class mass spectrogram automatic recognition system of world's common pesticides and chemical pollutant and method based on cloud platform |
| CN113671070A (en) * | 2021-07-30 | 2021-11-19 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | Establishment and application of high-throughput screening mass spectrum database for cosmetic safety risk substances |
| CN113340873A (en) * | 2021-08-09 | 2021-09-03 | 北京市疾病预防控制中心 | SERS system for simultaneously detecting multiple toxic substances |
| CN114047280A (en) * | 2021-10-21 | 2022-02-15 | 苏州药明康德新药开发有限公司 | Method for detecting content of non-volatile unknown substances in medical instrument leaching liquor |
| CN115015403A (en) * | 2022-04-08 | 2022-09-06 | 浙江大学 | Rapid, comprehensive and stable identification method for unknown poison |
| WO2023193323A1 (en) * | 2022-04-08 | 2023-10-12 | 浙江大学医学院附属第一医院 | Rapid, comprehensive and stable identification method for unknown toxicants |
| CN115248271A (en) * | 2022-06-07 | 2022-10-28 | 浙江理工大学绍兴生物医药研究院有限公司 | Qualitative analysis method for volatile components of salvia officinalis |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103823008B (en) | 2016-03-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103823008B (en) | Build the method that liquid chromatography-mass spectrography database detects unknown poisonous substance | |
| Wolfender et al. | Accelerating metabolite identification in natural product research: toward an ideal combination of liquid chromatography–high-resolution tandem mass spectrometry and NMR profiling, in silico databases, and chemometrics | |
| Turnipseed et al. | Wide-scope screening method for multiclass veterinary drug residues in fish, shrimp, and eel using liquid chromatography–quadrupole high-resolution mass spectrometry | |
| Deng et al. | Identification of chemical ingredients of peanut stems and leaves extracts using UPLC‐QTOF‐MS coupled with novel informatics UNIFI platform | |
| CN108593828A (en) | Blood plasma prepares the detection method of drug and toxic content in card | |
| Clark et al. | Interlaboratory comparison of untargeted mass spectrometry data uncovers underlying causes for variability | |
| CN101859305A (en) | Liquid chromatogram and mass spectrum database of common poisons and medicines | |
| López-Ruiz et al. | Metabolomics approaches for the determination of multiple contaminants in food | |
| Wu et al. | Comparison of data acquisition modes with Orbitrap high‐resolution mass spectrometry for targeted and non‐targeted residue screening in aquacultured eel | |
| Singh et al. | Quantitative determination of isoquinoline alkaloids and chlorogenic acid in Berberis species using ultra high performance liquid chromatography with hybrid triple quadrupole linear ion trap mass spectrometry | |
| Zhu et al. | Suspect screening and untargeted analysis of veterinary drugs in food by LC-HRMS: Application of background exclusion-dependent acquisition for retrospective analysis of unknown xenobiotics | |
| CN112903890A (en) | Method for identifying traditional Chinese medicine components in food based on high-resolution mass spectrometry technology | |
| Vacillotto et al. | A rapid and highly specific method to evaluate the presence of pyrrolizidine alkaloids in Borago officinalis seed oil | |
| Fuenffinger et al. | Evaluation of ion mobility spectrometry for the detection of mitragynine in kratom products | |
| Xu et al. | Determination of monosaccharides in Lycium barbarum fruit polysaccharide by an efficient UHPLC‐QTRAP‐MS/MS method | |
| CN106442772A (en) | Method for detecting and analyzing anticoagulant rodenticides in blood | |
| Kamble et al. | Quantitative estimation of gymnemagenin in Gymnema sylvestre extract and its marketed formulations using the HPLC–ESI–MS/MS method | |
| Singh et al. | Simultaneous determination of pyrroquinazoline alkaloids and flavonoids in Adhatoda beddomei and Adhatoda vasica and their marketed herbal formulations using ultra‐high‐performance liquid chromatography coupled with triple quadrupole linear ion trap mass spectrometry | |
| Rojano‐Delgado et al. | Ultrasound‐assisted Extraction with LC–TOF/MS Identification and LC–UV Determination of Imazamox and its Metabolites in Leaves of Wheat Plants | |
| Paracampo et al. | Chemotaxonomic study of Chrysobalanus icaco Linnaeus (Chrysobalanaceae) using ultra‐high performance liquid chromatography coupled with diode array detection fingerprint in combination with multivariate analysis | |
| Filipiak-Szok et al. | Simultaneous Determination of Isoquinoline Alkaloids in Medicinal Asiatic Plants by Ultrasound-Assisted Extraction and High-Performance Liquid Chromatography–Mass Spectrometry with Principal Component Analysis | |
| Luo et al. | Establishment of a High-Resolution Liquid Chromatography–Mass Spectrometry Spectral Library for Screening Toxic Natural Products | |
| Talebpour et al. | Monitoring of the insecticide trichlorfon by phosphorus-31 nuclear magnetic resonance (31P NMR) spectroscopy | |
| Ebrahimi et al. | 1HNMR-based discriminatory analysis of eurycoma longifolia from different locations and establishing a profile for primary metabolites identification and quassinoids quantification | |
| CN109444290B (en) | Construction method and detection method of UPLC (ultra performance liquid chromatography) characteristic map of plantain herb |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |