CN104880506B - The detection method of synthetic drug ingredient and its application in a kind of food - Google Patents
The detection method of synthetic drug ingredient and its application in a kind of food Download PDFInfo
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Abstract
The present invention provides a kind of detection methods of synthetic drug ingredient in food, carry out classification and Detection to the standard sample of synthetic drug ingredient to be checked the method includes (1) and establish standard database；(2) food samples are detected；(3) testing result is compared and is drawn a conclusion with standard database automatically by instrument.Analysis is completed to be no more than one minute.The method of the present invention without professional training, instrument is portable, operation sequence is simple, consumptive material is low-cost, detection speed is fast, health-care product superintendent office of base be can be used as in law enforcement field or professional testing agency's method that synthetic drug ingredient carries out rapid batch scalping in laboratory is to health products, its detection cycle will be greatly shortened, working efficiency is improved, testing cost is reduced.
Description
Technical field
The present invention relates to field of food safety, specifically, are related to a kind of detection method of synthetic drug ingredient in food
And its application.
Background technology
With the progress of society and economic development, the nutrition and health care effect of food is increasingly valued by people,
Simultaneously because rhythm of life is constantly accelerated, the crowd in sub-health state is on the increase, and is improved using health food and is adjusted
Bodily fuctions also become the trend of people's self health care.End in March, 2014, state food pharmaceuticals administration general bureau (CFDA)
The health food of examination ＆ approval has 14212, wherein national OTC 13493, import health food 719 (data source in
CFDA health foods database).Flourishing for health food brings huge society and economic effect to China's food service industry
Benefit, but since China's Health Food Industry Development is started late, the quality of enterprise is irregular, and market surveillance management system has waited
Kind, health food has been reported that due to illegally adding chemicals by the case where investigation repeatly.
To further strengthen health food supervision, it is non-that state food pharmaceuticals administration general bureau starts strike health food
The unlawful practices such as method production, illegal operation, illegal addition and illegal publicity." illegal addition " is common in two classes, Yi Leishi
Chemicals add, another kind of, are to be common in extract with inferior or other alternative materials, alternative materials.For illegal medicine
Object adds, and since health food is the product based on function, to show its validity, addition generally can be more in its effective concentration
The case where number is the micro level to constant, while its effect is shown, there is also compound additions for enhancing.The drug of addition is often
It is Common drugs, drug either pro-drug etc. of quitting listing；Situations such as there is also the crude products of addition drug.
Various regions Examined is shown, in slimming health food, the addition of sibutramine, three kinds of phenolphthalein, caffeine drugs
It is more serious；In hypoglycemic class health food, insoral, melbine, the addition of three kinds of drugs of glibenclamide are more tight
Weight；In alleviating physical fatigue class, silaenafil, the addition of two kinds of drugs of Tadalafei are more serious.
Therefore, foundation is more comprehensively quick, and accurately and reliably forbidden drug screening technique, to cope with speculating for criminal
Behavior is played the role of checking on conscientiously in links, can prevent and supervise health food to enter caused bad thing behind market
Part occurs, it is ensured that the safety of health food has important reality meaning to protecting the just rights and interests and health of consumer
Justice.
In order to fast and effeciently detect the chemicals illegally added in health food, domestic and international researcher carries out
A large amount of research, it was recently reported that many relevant detection techniques, mainstream technology are still laboratory common detection methods, such as：Thin layer
Chromatography (TLC), high performance liquid chromatography (HPLC), liquid chromatograph mass spectrography (LC-MS), infrared and near infrared spectroscopy (IR/
NIR), nuclear magnetic resonance method (NMR), capillary electrophoresis (CE) etc..In previous supervision law practising, traditional inspection is utilized
Though method accuracy, high sensitivity, complicated for operation, time-consuming, of high cost.For example, depending on large-scale instrument such as mass spectrum, chromatography
Although lab analysis detection technique it is accurate, reliable, there is the period it is long, strongly professional, costly the deficiencies of, it is difficult to and
When, rapidly monitor the safe condition of food, be not suitable for the screening for carrying out a large amount of samples, the situation of retardation problem sample is investigated
And discovery.Therefore quicker, easy, at low cost, time-consuming short rapid detection method is used food more and more
In the work of product safety supervision management, larger efficiency has been played, an important technology hand is provided quickly to pinpoint the problems
Section.The appearance of these pocket equipment enables Fast Detection Technique more to adapt to the requirement of Site Detection, general quickly to detect
And guarantee is provided, it is provided a convenient especially for base reviewer.
Ion mobility spectrometry (IMS) technology originates from nineteen sixties as a kind of trace Detection Techniques, early stage
Patent (US 3699333 and 4777363) has carried out detailed description to this technology.Since IMS apparatus structures are simple, detection
High sensitivity (detection limit reaches pg-ng grades), is particularly suitable for the trace detection of some volatile organic compounds.More than past 20
Nian Li, domestic and international multiple academic institutions and company have carried out a large amount of research work, especially needle to the practical application of IMS technologies
To the fields such as illicit drugs inspection, explosive detection, chemical warfare agent detection, detection of biological field agents application (RU2288459,
WO2004018994, US6477907, CA2043825, US2005278142, KR20020017491 etc.), and obtain considerable
Development, at the same be also extended to environment measuring (EP1006372, US6969851 etc.), industrial stokehold (WO2004016850,
US2002121349, CA2097269, CA2069029, CA2009062, EP0683392 etc.), it is biomedical (DE10339015,
US6365339, USH1563H, US4988628 etc.), the multiple fields such as Food Monitoring (DE10339014, EP1233267 etc.).
Application (food security quality testing in terms of IMS technologies illegally add chemicals in health food at present
Report, 2014,5 (9):It 2657-2662) describes a kind of detected in slimming health food using IMS technologies and illegally adds drug
Method.But the detection method for not mentioning phenolphthalein in the method for the displosure, for occupy weight-reducing class health food in illegally add compared with
For serious chemicals, there are certain to fail to report risk.
Invention content
It is an object of the present invention to provide a kind of detection methods of synthetic drug ingredient in food；
The detection of synthetic drug ingredient that another object of the present invention is to provide the detection methods in food is answered
With.
In order to achieve the above object, on the one hand, it is described the present invention provides a kind of detection method of synthetic drug ingredient in food
Method is detected the standard sample of synthetic drug ingredient to be checked and establishes standard database respectively including (1)；(2) to food
Sample is detected；(3) testing result is compared and is drawn a conclusion with standard database automatically by instrument.
The present invention is detected and is compared automatically using instrument, and the analysis deadline is within 1 minute.
According to the preferred embodiment of the present invention, the input mode of the detection selects direct sample feeding method.
According to the preferred embodiment of the present invention, the direct sample feeding method includes carrying out unlap to food samples
Pre-treatment, by the wiping of treated food samples on sampling carrier and being inserted into the instrument injection port of detection and examine
It surveys.According to the preferred embodiment of the present invention, the method is detected using ionic migration spectrometer, ionic migration spectrometer
Testing conditions include：Sampling line number is 40-100, sample introduction pump discharge 0-0.6L/min, migration pump discharge 0.6-0.8L/min；From
The ion gate Voltage Pulse Width of sub- mobility spectrometer is 300-800 μ s；
The testing conditions of further preferred ionic migration spectrometer wherein of the invention include：It is 50 to sample line number, sampling pump
Flow 0L/min, migration pump discharge 0.6L/min.
According to the preferred embodiment of the present invention, the testing conditions of ionic migration spectrometer further include：Positive transfer tube temperature degree is set
It is set to 130-190 DEG C, at 100-150 DEG C, injector temperature is arranged at 80-220 DEG C negative transfer pipe temperature setting.
The wherein present invention further preferably testing conditions of ionic migration spectrometer further include：Positive transfer tube temperature degree is set as
170 DEG C, at 130 DEG C, injector temperature is arranged at 210 DEG C negative transfer pipe temperature setting.
According to the preferred embodiment of the present invention, the clean conditions of ionic migration spectrometer further include：Sampling pump blowback flow
0-0.6L/min, migration pump discharge are 0.6-0.8L/min.
The wherein present invention further preferably clean conditions of ionic migration spectrometer further include：Sampling pump blowback flow 0.6L/
Min, migration pump discharge are 0.6L/min.
Wherein it is understood that when sampling pump is in sample introduction state, pump runs well；When in clean conditions,
Sampling pump can be reversed operating, by blowback to be cleaned to equipment.Therefore, when in clean conditions, sampling pump can also claim
For blowback pump.
According to the preferred embodiment of the present invention, the clean conditions of ionic migration spectrometer further include：Positive transfer tube temperature degree is set
It is set to 130-190 DEG C, at 100-150 DEG C, injector temperature is arranged at 80-220 DEG C negative transfer pipe temperature setting, samples line number
40-100 items.
The wherein present invention further preferably clean conditions of ionic migration spectrometer further include：Positive transfer tube temperature degree is set as
170 DEG C, at 130 DEG C, injector temperature is arranged at 210 DEG C negative transfer pipe temperature setting, samples line number 50.
According to the preferred embodiment of the present invention, the ion gate Voltage Pulse Width of ionic migration spectrometer is 380 μ s.
According to the preferred embodiment of the present invention, when containing aloe, lotus leaf, certainly in step (2) the food samples ingredient
When one or more in pine torch, rhizoma alismatis, lactose and maltose, described be detected to food samples is come to carry out detection twice
Determine final analysis result, at 80-110 DEG C, second of injector temperature is arranged at 210 DEG C the setting of first time injector temperature；
It is preferred that first time injector temperature is set as 100 DEG C；
Wherein the present invention further preferably：The setting of first time injector temperature is at 100 DEG C, second of injector temperature
It is arranged at 210 DEG C.
According to the preferred embodiment of the present invention, wherein step (1) includes：By the standard sample of synthetic drug ingredient to be checked
Be configured to the stock solution of 1mg/mL respectively, and be diluted to suitable concentration and obtain the standard solution of experiment, take standard solution into
Sample obtains the ion transfer spectrogram of standard sample, according to the ion transfer spectrogram that standard solution obtains under various concentration, by synthesis
The type of drug establishes the standard database of each synthetic drug to be checked.
According to the preferred embodiment of the present invention, wherein step (1) includes the standard under the various concentration after taking 1 μ L dilutions
Solution sample introduction.
According to the preferred embodiment of the present invention, wherein step (1) includes measuring the ion of synthetic drug ingredient to be checked
Reach detector transit time and peak intensity, in ionic migration spectrometer be arranged synthetic drug ingredient feature transit time with
And alarm threshold value, establish the standard database of all kinds of synthetic drug ingredients to be checked.
According to the preferred embodiment of the present invention, wherein step (2) includes：To food samples pre-treatment, by treated
Food samples wiping in sampling carrier on and be inserted into ionic migration spectrometer injection port, the sample of instrument sample and obtain
Ion transfer spectrogram.
According to the preferred embodiment of the present invention, wherein step (2) can be according to sample to the pre-treatment of food samples
Type is selected with concrete condition, and for example tablet form health food need to pass through removal sugar-coat and grind, capsule and soft-capsule type
Health food need to remove the peel processing, and teas health food need to stay stationery to pack, then micro-example wiping is carried in sampling by treated
On body (for teas health food, sampling carrier wipes its stationery package interior remnants).
According to the preferred embodiment of the present invention, wherein step (3) includes：If in the ion transfer spectrogram of food samples
There are the peak intensities that goes out at the feature transit time of synthetic drug and this feature peak to be greater than or equal to appearance intensity threshold, it is determined that
Food samples are positive and generate pre-warning signal；And if the spy of synthetic drug is not present in the ion transfer spectrogram of food samples
Sign peak or there are the peak intensities that goes out at the characteristic peak of synthetic drug but this feature peak to be less than the appearance intensity threshold, it is determined that
Food samples are feminine gender；And it can going out according to the characteristic peak for corresponding to synthetic drug in the weight and ion transfer spectrogram of food samples
Peak intensity sxemiquantitative estimates the concentration of synthetic drug in food samples.
Wherein it is understood that synthetic drug of the present invention refers to artificial synthesized drug.And it may further
What is understood is the ingredient for forbidding addition in the concerned countries of the food detected or local regulation.
According to the present invention, it is only necessary to take simple directly wiping sample introduction pre-treatment step, sample be wiped straight on carrier
The mode of sample is tapped into, can realize that the quick detection to 81 kinds of synthetic drug ingredients, detection are limited to ppb-ppm respectively in 1 minute
Grade.This method without professional training, instrument is portable, operation sequence is simple, consumptive material is low-cost, detection speed is fast, can be used as base
Layer health-care product superintendent office law enforcement field or professional testing agency in laboratory is to health products synthetic drug ingredient into
The method of row rapid batch scalping will greatly shorten its detection cycle, improve working efficiency, reduce testing cost.
According to the preferred embodiment of the present invention, wherein the sample is health food.
According to the preferred embodiment of the present invention, for part slimming health food using detection (postsearch screening side twice
Method), i.e.,：For in product containing aloe, lotus leaf, cassia seed, rhizoma alismatis, lactose, maltose health food, select injection port temperature
Degree carries out screening for 100 DEG C of testing conditions, reports phenomenon by mistake caused by volatilizing to avoid interference component, then increase temperature, utilizes
The screening again of 210 DEG C of testing conditions avoids that failing to report for caffeine or phenolphthalein occurs.
According to a preferred embodiment of the invention, the present invention can be more specifically：
According to the arbitrary detection method before the present invention, the method is detected using ionic migration spectrometer,
The testing conditions of ionic migration spectrometer include：It is 50, sample introduction pump discharge 0L/min, migration pump discharge 0.6L/min to sample line number.
The testing conditions of preferred ion mobility spectrometer wherein of the present invention further include：Positive transfer tube temperature degree is set as 170 DEG C, bears
At 130 DEG C, injector temperature is arranged at 210 DEG C migration tube temperature setting.
The clean conditions of preferred ion mobility spectrometer wherein of the present invention include：Sampling pump blowback flow 0.6L/min, migration
Pump discharge is 0.6L/min.
The clean conditions of preferred ion mobility spectrometer wherein of the present invention further include：Positive transfer tube temperature degree is set as 170 DEG C, bears
At 130 DEG C, injector temperature is arranged at 210 DEG C migration tube temperature setting, samples line number 50.
The ion gate Voltage Pulse Width of preferred ion mobility spectrometer wherein of the present invention is 380 μ s.
Wherein the present invention preferably when in step (2) the food samples ingredient contain aloe, lotus leaf, cassia seed, rhizoma alismatis, breast
When one or more in sugar and maltose, described be detected to food samples determines final analysis detect twice
As a result, the setting of first time injector temperature is at 100 DEG C, second of injector temperature is arranged at 210 DEG C.
On the other hand, the detection of synthetic drug ingredient that the present invention also provides the detection methods in food is answered
With.
According to the preferred embodiment of the present invention, the food is health food.
In conclusion the present invention provides a kind of detection method of synthetic drug ingredient in food and its applications.The present invention
Detection method have the following advantages that：
Synthetic drug ingredient in health products is used for quickly detecting using Ion mobility spectrometry the present invention provides a kind of
Method, can by using simple directly sample feeding pre-treatment step, efficiently easily realize to 81 kinds of synthetic drugs at
The quick detection and acousto-optic early warning divided, for detection time less than 1 minute, method detection was limited to ppb-ppm grades, had very low false sun
Property (≤15%) and false negative rate (≤1%), can be used as the rapid screening technology for these synthetic drug ingredients, if must
It wants, only needs to carry out accurate qualitative and quantitative analysis to the sample for generating alarm signal in practical application.With existing disclosed inspection
Survey method compares (food security quality testing journal, 2014,5 (9):2657-2662) there is following advantage：
(1) direct sample feeding mode saves detection time, breaks away from laboratory routine experiment device such as scroll machine, ultrasound
Cleaning machine, centrifuge.Direct sample feeding method is compared with simple solvent extracting process, can save pre-treatment time 15-20 point
Clock or so/sample can save detection time, break away from sample pre-treatments for Rapid food safety inspection instrument device, have huge
Big advantage.
(2) sampling line number increases, and for some molecules that ionization rate is slow, sampling line number, which increases, can effectively avoid detection
Imperfection, improve accuracy in detection.
(3) instrument parameter intermediate ion gate voltage pulse width (ion gate opening time) is broadening, improves instrumental sensitivity.
(4) cleaning mode increases sampling pump blowback flow.It, can after sampling pump blowback flow is opened under instrument cleaning mode
Inverted draft purging injection port semi-permeable membrane and sampling device are provided, make the sample carryover being present on injection port and semi-permeable membrane as early as possible
Removal is played the role of improving cleaning speed, reinforces cleaning dynamics, residual for substance to save the experiment assay intervals time
More serious sample is stayed, assay intervals 13-15min or so can be saved by opening sampling pump blowback.
(5) migration pump discharge reduces, when instrument detection signal when flow is reduced to 0.6L/min with flow is 0.8L/min
Detection signal compared to not significantly decreasing, and when flow is 0.6L/min instrument mixing screening capacity by original primary
At most can 6 kinds of synthetic drug ingredients of screening be increased to can 10 kinds of synthetic drug ingredients of a screening, improve instrument separation effect
Rate.
(6) it is directed to part slimming health food and uses postsearch screening pattern, can detect addition relatively conventional in the market
Phenolphthalein.For in product composition containing aloe, lotus leaf, cassia seed, rhizoma alismatis, lactose, maltose health food, select injection port
Temperature is after 100 DEG C of testing conditions screening avoids wrong report, then increases temperature, using the screening again of 210 DEG C of testing conditions, with
Avoid occurring caffeine or phenolphthalein fails to report police.Other slimming health foods then only need to be under the testing conditions of 210 DEG C of injection port
It carries out, includes the health food to unknown packaging sample.
(7) due to being not necessarily to external gas source and independent display, equipment instrument is small and exquisite portable, is convenient for on-the-spot test, analysis
Speed is fast.Instrument is operated without specialty background personnel, and consumptive material is seldom, and operating cost is low, particularly suitable for law enforcement agency of base and
Profession testing agencies at different levels carry out the general inspection primary dcreening operation of high-volume health products samples, in actual operation can be with the confirmations such as UPLC-MS
Method is combined, and is realized from quantitative quick and precisely detection is just sieved to, to further strengthening health food security control, Quan Mianti
The Ability of emergency management of high food safety affair has great importance.
Description of the drawings
Fig. 1 is ionic migration spectrometer composition and principle sketch.
Fig. 2 (a) and Fig. 2 (b) is the improved detection comparison diagram of sample feeding mode (holotype and negative mode).
Fig. 3 (a) and Fig. 3 (b) is that the improved detection comparison diagram of line number (holotype and negative mode) is sampled in instrument parameter.
Fig. 4-1 (a), Fig. 4-1 (b), Fig. 4-2 and Fig. 4-3 are instrument parameter intermediate ion gate voltage pulse widths to instrument spirit
The influence diagram of sensitivity.
Fig. 5 (a) and Fig. 5 (b) is sampling pump blowback flow switch under cleaning mode on clean influence comparison diagram (holotype
And negative mode).
Fig. 6-1 (a), Fig. 6-1 (b), Fig. 6-1 (c) and Fig. 6-1 (d) are to migrate pump discharge in instrument parameter to improve to instrument
The influence comparison diagram of resolution capability.
Fig. 6-2 (a), Fig. 6-2 (b), Fig. 6-2 (c) and Fig. 6-2 (d) are that instrument after pump discharge is improved is migrated in instrument parameter
Mixing screening capacity comparison diagram.
Fig. 6-3 (a), Fig. 6-3 (b) be migrated in instrument parameter influence datagram of the pump discharge to ion signal intensity and
Migrate influence datagram of the pump discharge to instrument resolution capability.
Fig. 6-4 (a), Fig. 6-4 (b) are the influences for migrating pump discharge in instrument parameter and cleaning sample carryover ability to instrument.
Fig. 7 is the spectrogram obtained using the practical commercially available health products aloe capsule for easying astriction of UPLC-MS methods detection.
Fig. 8-1 (a), Fig. 8-1 (b) are to detect practical city using ionic migration spectrometer using the method provided in embodiment
Sell the spectrum that the positive and negative pattern ion mobility spectrometry instrument Orgin8.6 softwares that health products aloe capsule for easying astriction obtains are handled
Figure.
Fig. 9 is to be good for the spectrogram that clear good clear smooth capsule obtains again using the practical commercially available health products soup minister of UPLC-MS methods detection.
Figure 10-1 (a), Figure 10-1 (b) are to detect practical city using the method provided in embodiment ionic migration spectrometer
Health products soup minister positive and negative 8.6 softwares of pattern ion mobility spectrometry instrument Orgin that strong clear good clear smooth capsule obtains again are sold to handle
The spectrogram arrived.
Specific implementation mode
Below by way of the advantageous effect of the specific embodiment implementation process that the present invention will be described in detail and generation, it is intended to which help is read
Reader more fully understand the present invention essence and feature, not as to this case can practical range restriction.
Fig. 1 is the composition and principle schematic of a kind of ionic migration spectrometer of specific implementation mode according to the present invention.Institute
It can be traditional uniform field ion mobility spectrometry equipment to state ionic migration spectrometer 1, as shown in Figure 1, one end has injection port 2,
The air sample of the atmosphere containing determinand can be acquired or the sampling carrier for being collected into solid particle samples is introduced into instrument, injection port end
Hot parser is set, for the solid particle samples on heating and gasifying sampling carrier.There is selection to penetrate for setting one in injection port
The semi-permeable membrane 3 of property, by instrument internal with and the sampling device that communicates of external environment separate.By different input modes by injection port
The 2 gaseous state measured matter molecules introduced are brought by air stream to semi-permeable membrane under the action of sampling pump 10, by the screening of film
Effect fails then to be discharged by sampling pump 10 through the component of film into the core element transference tube 4 in instrument.Migration tube 4
7 two parts of ionization reaction zone 6 and migration area are separated by the ion gate 5 that can periodically open.By in ring-type in migration area
Voltage is imposed on electrode slice 8 to provide equally distributed electric field.In the ionization area of transference tube, determinand molecule is ionized simultaneously
Ion cluster is formed, when ion gate is opened, these ion clusters enter migration area under the action of electric field and continue the work in electric field
Advanced with lower migration.In migration area, the factors such as the migration velocity of ion cluster and its quality, volume, charge are related, therefore different
Ion cluster reach positioned at migration area end detector 9 time it is different, by detecting the faint arteries and veins come self-detector
It rushes electric current and its arrival time, and it is matched with standard substance library, so that it may to judge the type of substance.After instrument
The migration airflow direction being introduced into and ion motion direction are held on the contrary, being exported close at the position of ion gate in ionization room, is being followed
Under the impetus of ring air pump 11, after entering migration area as migration air-flow by the gas part after 12 purge drying of filter
Portion, part is then by may include that the gas circuit of dopant source 13 enters ionization reaction zone.The electric polarity of migration area 7 determines the inspection of instrument
Survey pattern, when polarity is timing, the anion that ionization area 6 generates is introduced in migration area 7 and is detached and detected, and obtains negative norm
Formula ion transfer spectrogram, conversely, when polarity is negative, cation that ionization area 6 generates be introduced in migration area 7 carry out separation and
Detection, obtains holotype ion transfer spectrogram.Using the quick alternate single migration tube of polarity or opposite polarity double migration tubes
Design method obtains holotype and negative mode ion transfer spectrogram, it can be achieved that being detected while positive and negative ion.
Method according to an embodiment of the invention for being used for quickly detecting to the synthetic drug ingredient in health products can
To include using ionic migration spectrometer to the foundation in the synthetic drug ingredient standard substance library in health products and to health products to be measured
Detection two parts of sample.
In standard substance established part of the library, to save procurement criteria material cost, to the standard of 81 kinds of synthetic drug ingredients
Substance takes organic solvent to extract mode, then extract liquor is added drop-wise on sampling carrier and is inserted into ionic migration spectrometer sample introduction
The mode of mouth, the method established to the synthetic drug ingredient standard substance library in health products include the following steps：
(1) standard items that required all kinds of Western medicine substances are accurately weighed using the electronic balance of ten a ten thousandths, use matter respectively
Spectrum level absolute methanol dissolves and is settled to 10mL volumetric flasks, is configured to the standard solution of 1mg/mL, and 4 DEG C of refrigerations are spare.When use
The standard solution prepared is diluted to suitable concentration step by step with absolute methanol, 1 μ L standard solution is taken to be added drop-wise to special sampling carrier
Upper sample introduction obtains corresponding ion transfer spectrogram.The ion for measuring different Western medicine substances reaches time and the peak intensity of detector,
Record the signal strength that its content corresponds to peak.Same Western medicine standard substance record respectively under various concentration corresponding transit time and
Peak intensity determines feature peak position and sensitivity section, and going out peak intensity according to chaff interferent that may be present in anima determines inspection
Threshold value is surveyed, the standard substance library of the synthetic drug ingredient is established.
Classification inspection is realized in the screening part of synthetic drug ingredient in health food to the health food of existing packaging brand
Screening is surveyed, the blind sieve of unknown health food can be carried out and repeat screening by different classifications, to avoid to 81 kinds of synthetic drugs
Report the presence of phenomenon in the detection process of ingredient by mistake.The method of synthetic drug ingredient screening in health products is included the following steps
(2)：Input mode selects direct sample feeding method, and wherein tablet Biscuits needs to grind removes sugar-coat, glue if having sugar-coat
Capsule and soft capsule class need to remove the peel, and teas and electuary class go outer packing, drinks or injector for oral use to extract 1 μ L sample introductions.
Little power particle is taken to be carried in (teas and electuary class sampling carrier wipe outer packing) on sampling carrier, then by sampling
Body is sent to ion mobility spectrometry and is analyzed, and obtains the detection signal of transit time and corresponding peak intensity；And it is obtained with the step 1
The appearance time of the synthetic drug ingredient obtained is compared, if existed in the ion transfer spectrogram of health products sample to be measured illegal
The characteristic peak of the Western medicine of addition and the detection threshold value for going out peak intensity and being greater than or equal to step 1) setting at this feature peak, it is determined that
The sample of health products is positive and generates pre-warning signal；And if there is no illegal in the ion transfer spectrogram of the sample of health products
The characteristic peak of the Western medicine of addition or the characteristic peak that there is the Western medicine illegally added, but the peak intensity that goes out at this feature peak is less than institute
State appearance intensity threshold, it is determined that the sample of health products is feminine gender.It, will be in ion transfer spectrogram according to the weight of health products sample
The detection signal that peak intensity is obtained with examination criteria sample in step 1) that goes out of the characteristic peak of corresponding synthetic drug ingredient is compared
It is right, can sxemiquantitative estimate the concentration of synthetic drug ingredient in health products sample.
Before the operation of the step 2, different samples are needed to carry out different pretreatments, such as tablet and powder, cake
It does, needs mortar grinder at uniform powder, there is the removal sugar-coat of sugar-coat；For conventional capsule, coat is needed；For soft
Capsule needs to extract interior liquid；For teas, solid granules or coffee, it can directly utilize the residual powder in outer packing；For mouth
Liquid or drinks are taken, needs to remove outsourcing bottling with being added drop-wise on sampling carrier after 1 μ L of injector extraction, is inserted into after solvent flashing
To instrument injection port.
A kind of embodiment according to the present invention, the appearance intensity threshold of synthetic drug ingredient and right in determining health products
During health products sample to be measured is detected, the sample introduction carrier is identical, material include sheet metal or sieve, into
Sample paper or polytetrafluoro thin slice；The extraction organic solvent includes the acetone or methanol that can dissolve the high substance of volatility.
The health products include weight-reducing class, auxiliary hyperglycemic class, adjust immunity class, alleviate physical fatigue class, auxiliary drop
Blood-lipoids, aided blood pressure-lowering class improve sleep class, tonifying kidney and strengthening yang class health products, wherein may contain in weight-reducing class health products
Synthetic drug ingredient includes ephedrine, d-pseudo-ephedrine, caffeine, Bupropion, fenfluramine, phenylpropanolamine, benzocainum, west
Cloth Qu Ming, single demethylated sibutramine, dinor- sibutramine, theophylline, Prozac, Sertraline, synephrine, Clenbuterol,
Citalopram, frusemide, spirolactone, bumetanide, chlorothiazide, acetazolamide, Torasemide, Topiramate, Nandrolone Phenylpropionate, three
Ammonia pteridine, acarbose, benfluorex, Yi Nita acid, indapamide, west are for Li Sita, Rimonabant, phenolphthalein, rheum emodin, azoles
Silt amine, bendroflumethiazide；The synthetic drug ingredient that may contain in auxiliary hyperglycemic class health products includes melbine, benzene second pair
Guanidine, glibenclamide, Glimepiride, Glipizide, gliclazide, orinase, Pioglitazone, gliquidone, Rosiglitazone,
Repaglinide；It adjusts immunity, alleviate the synthetic drug that may contain in physical fatigue class, tonifying kidney and strengthening yang class health products into subpackage
Include pseudo- Vardenafil, Vardenafil, silaenafil, that not silaenafil, person of outstanding talent not silaenafil, hydroxyl person of outstanding talent not silaenafil, ammonia
Base Tadalafei, Tadalafei, Acctildenafil, that Acctildenafil, that is non-on thio Chinese mugwort ground；Assisting may in reducing blood lipid class health products
The synthetic drug ingredient contained includes Lovastatin, Simvastatin, niacin；The conjunction that may contain in aided blood pressure-lowering class health products
Include captopril, nifedipine, Hydrochioro, clonidine, prazosin, reserpine, atenolol at drug ingedient；Improvement is slept
The synthetic drug ingredient that may contain in dormancy class health products includes diazepam, Lorazepam, Clonazepam, nitrazepam, Ao Shaxi
It dissolves, chlordiazepoxide, triazolam, estazolam, alprazolam, midazolam maleate, barbital, amytal, Si Keba ratio
Appropriate sodium, phenobarbital.
Fig. 2 (a) to Figure 10-1 (b) is provided some and is given to the present invention using the experiment spectrogram that ionic migration spectrometer obtains
Illustrate, the operating parameter of instrument is：
(1) testing conditions：To purify air as carrier gas and migration gas, positive transfer tube temperature degree is set as 170 degree, negative transfer
At 130 degree, injector temperature is arranged at 210 degree pipe temperature setting, samples line number 50, sample introduction pump discharge 0L/min, migration pump
Flow 0.6L/min.Wherein injector temperature can quickly be adjusted according to health products sample class and main component, to eliminate
The influence of matrix interference object.
(2) clean conditions：To purify air as carrier gas and migration gas, positive transfer tube temperature degree is set as 170 degree, negative transfer
At 130 degree, injector temperature is arranged at 210 degree pipe temperature setting, sampling line number 50, sampling pump blowback flow 0.6L/min,
Migrate pump discharge 0.6L/min.
Fig. 2 (a) and Fig. 2 (b) is the improved detection pair of the sample feeding mode by taking the strange board show appearance slimming capsule in river as an example
Than figure.1# is to obtain sample solution using solvent extraction, weighs a dose of health products, fixed with 50mL absolute methanols
Hold, be vortexed, set aside for use after ultrasound, wherein tablet needs to grind, and capsule and soft capsule class need to remove the peel, and teas need to remove stationery packet
Dress.The solvent samples solution after 1 μ L extractions is taken to be sent to the IMS figures that ion mobility spectrometry is analyzed.2# is direct sample
The IMS figures that input mode obtains, wherein tablet need to remove sugar-coat, and capsule and soft capsule class need to remove the peel, drinks, oral solution class
1 μ L are directly extracted, teas need to go stationery to pack.Wherein horizontal axis is transit time (millisecond), and the longitudinal axis is the intensity (milli of ion signal
Volt).Holotype and the bright instrument obtained using organic solvent extracting process and using direct sample feeding method of negative mode chart
Testing result is not much different, and directly sample feeding method can more effectively save detection time, and eliminates the reliance on laboratory
Device such as scroll machine, supersonic cleaning machine, centrifuge can be more applicable for spot sampling check use.Fig. 2 (a) is holotype, Fig. 2
(b) it is negative mode.
Fig. 3 (a) and Fig. 3 (b) be sampled in instrument parameter the improved detection comparison diagram of line number (with standard substance west that
For non-).1# is the IMS figures that Instrumental Analysis obtains when sampling line number 30.Instrumental Analysis obtains when 2# is sampling line number 50
IMS figure.Wherein horizontal axis is transit time (millisecond), and the longitudinal axis is the intensity (millivolt) of ion signal.Holotype and negative mode figure
Show that sampling line number increases that rear detection result is more acurrate, wherein the characteristic peak of silaenafil is 14.13 ± 0.1.Fig. 3 (a) is just
Pattern, Fig. 3 (b) are negative mode.
Fig. 4-1 (a), Fig. 4-1 (b), Fig. 4-2 and Fig. 4-3 illustrate ion gate voltage pulse by taking standard substance phenolphthalein as an example
Influence of the width (i.e. ion gate opening time) to instrumental sensitivity.1# opens for ion gate in Fig. 4-1 (a), Fig. 4-1 (b)
The detection spectrogram of phenolphthalein standard substance when door 300 μ s of time.The inspection of phenolphthalein standard substance when 2# is 380 μ s of ion gate opening time
Survey spectrogram.Wherein horizontal axis is transit time (millisecond), and the longitudinal axis is the intensity (millivolt) of ion signal.The holotype and negative norm of phenolphthalein
After the spectrogram of formula shows that the extension of ion gate opening time is 380 μ s, detection sensitivity is significantly improved, wherein the feature of phenolphthalein
Peak is 11.23ms ± 0.1.Fig. 4-1 (a) is holotype, and Fig. 4-1 (b) is negative mode.
Instrument detection sensitivity and resolution ratio are related with ion fence gate pulse width.Fig. 4-2 shows different ions portal vein
Influence of the width to migration tube signal strength is rushed, when ion fence gate pulse width is smaller, signal strength is with ion fence gate pulse
The increase of width and become strong；When ion fence gate pulse width increases to about 380 μ s, signal strength is by kept stable, no
Change again with the variation of ion fence gate pulse width.Fig. 4-3 shows during entire ion fence gate pulse width variation,
Half-peak breadth FWHM is then constantly broadened with the increase of ion fence gate pulse width, and resolution ratio declines.
Therefore, ion gatewidth is considered to the resolution ratio of drift tube and the influence of sensitivity, pulse width one
As to be chosen to be 300 μ s or so more suitable, for the actually detected situation of 81 kinds of synthetic drug ingredients, select 380 μ s as from
Cervical orifice of uterus pulse width.
Fig. 5 (a) and Fig. 5 (b) is for sampling pump blowback flow switch under cleaning mode on clean influence comparison diagram (with Kang Xing
For board Wei Lening soft capsules).The instrument cleaning situation IMS figures of 1# is sampling pump blowback flow when being 0 cleaning mode 3min.2#
The instrument cleaning situation IMS figures of cleaning mode 3min when for sampling pump blowback flow being 0.6L/min.When wherein horizontal axis is migration
Between (millisecond), the longitudinal axis is the intensity (millivolt) of ion signal.Holotype and negative mode chart are bright, in removal sample after detection
Sampling pump blowback switch has a major impact cleaning during residual.Open sampling pump blowback after can effectively shorten cleaning when
Between, rapidly to carry out the detection of next sample to be tested.Fig. 5 (a) is holotype, and Fig. 5 (b) is negative mode.
By Fig. 6-1 (a), Fig. 6-1 (b), Fig. 6-1 (c) and Fig. 6-1 (d) with sibutramine, the western cloth of-N-N- dinor-s
Illustrate to migrate the improved influence of pump discharge in instrument parameter for Qu Ming, phenolphthalein.It is double that 1# represents sibutramine, 2# representatives-N-N-
Demethylated sibutramine, 3# represent phenolphthalein.
Wherein Fig. 6-1 (a), Fig. 6-1 (b), Fig. 6-1 (c) and Fig. 6-1 (d) show that migrating pump discharge size differentiates instrument
Ability has a certain impact, and migration pump discharge can obviously distinguish sibutramine ,-N-N- dinor-s after changing into 0.6L/min
Sibutramine, phenolphthalein, the phenomenon that avoiding reporting by mistake or failing to report in detection process.Wherein Fig. 6-1 (a), Fig. 6-1 (b) be expressed as 1#,
The IMS spectrograms of 2#, 3# positive negative mode when migrating pump discharge and being 0.8L/min.Fig. 6-1 (c) and Fig. 6-1 (d) be expressed as 1#, 2#,
The IMS spectrograms of 3# positive negative modes when migrating pump discharge and being 0.6L/min.
After Fig. 6-2 (a), Fig. 6-2 (b), Fig. 6-2 (c) and Fig. 6-2 (d) show that migrating pump discharge changes into 0.6L/min,
Instrument is by most can illegal addition (food security quality testing journal, 2014,5 (9) of 6 kinds of screening simultaneously:2657-2662) change
At at most 10 kinds of screening simultaneously can illegally add, the detection accuracy of instrument is improved.Sample serial number see the table below 1.
1 Fig. 6-2 (c) of table and Fig. 6-2 (d) serial number names
| Sample number | Sample ID | Holotype peak position (ms) | Negative mode peak position (ms) |
| 1# | Caffeine | 8.73ms±0.1 | |
| 2# | Theophylline | 11.12ms±0.1 | |
| 3# | Fenfluramine | 9.67ms±0.1 | |
| 4# | Citalopram hydrobromate | 12.02ms±0.1 | |
| 5# | Ephedrine hydrochloride | 8.46ms±0.1 | |
| 6# | Sibutramine hydrochloride | 11.17ms±0.1 | |
| 7# | Hydrochloric acid-N-N- dinor- sibutramines | 11.45ms±0.1 | |
| 8# | Phenolphthalein | 11.23ms ± 0.1 (main peak) | 12.58ms±0.1 |
| 9# | Frusemide | 6.48ms±0.1 | 7.06ms ± 0.1 (main peak) |
| 10# | Rheum emodin | 14.59ms±0.1 | 10.81ms ± 0.1 (main peak) |
Fig. 6-2 (a), Fig. 6-2 (b), which give, to be detected with ionic migration spectrometer using the method provided in embodiment
The ion transfer spectrogram arrived, Fig. 6-2 (a), Fig. 6-2 (b) are the positive and negative mould that the anima without containing synthetic drug ingredient obtains
Formula ion transfer spectrogram；Fig. 6-2 (c) and Fig. 6-2 (d) be that adding for 10 kinds of synthetic drug ingredients is added in above-mentioned anima
The analysis result that standard specimen product obtain is superimposed positive and negative pattern ion transfer spectrogram, by two Fig. 6-2 (a), Fig. 6-2 (c) holotype spectrums
Figure and two Fig. 6-2 (b), Fig. 6-2 (d) negative mode spectrograms are compared respectively, it can be seen that by the way that rational threshold value is arranged,
This method can delicately detect 10 kinds of synthetic drug ingredients of a concentration of ppb-ppm.
Fig. 6-3 (a) and Fig. 6-3 (b) has studied the migration pump discharge for being suitble to 81 kinds of synthetic drug ingredients of detection.Fig. 6-3 (a)
By taking phenolphthalein is in the response signal under holotype as an example, ordinate is Ion response signal (millivolt), and abscissa is migration pump discharge
(L/min).By in figure it is found that response signal overall has the tendency that dying down with increases of migration pump discharge.
Fig. 6-3 (b) by-N-N- dinor-s sibutramine, phenolphthalein holotype feature transit time for, ordinate is
The two transit time is poor, abscissa be migration pump discharge, by figure it is found that migration pump discharge 0.1L/min-0.6L/min it
Between when, can obviously distinguish-N-N- dinor-s sibutramine, phenolphthalein.
In order to improve the resolution capability and ion signal intensity of instrument, from Fig. 6-3 (a) and Fig. 6-3 (b) it is found that should select
0.1L/min is selected, this flow can reach preferable effect for 81 kinds of synthetic drug ingredient these chemical substances, but for food
Product matrix itself, such as grease, sucrose substance, flow is small, these substances can be caused to be trapped in instrument, not volatile.
By taking industrial board fish oil soft capsule as an example, migration pump discharge is 0.1L/min by Fig. 6-4 (a) and Fig. 6-4 (b), and 1# is inspection
The ion transfer spectrogram that sample obtains；2# is to open sampling pump blowback flow 0.1L/min, cleans sample carryover after ten minutes,
The ion transfer spectrogram that blank assay obtains；Fig. 6-4 (a) is holotype, and Fig. 6-4 (b) is negative mode.As can be seen from Figure,
If sampling pump blowback flow also selects selection 0.1L/min, the oil in the edible substrates contained for sample itself such as soft capsule
Clean effect is then not achieved in fat.
In conclusion instrument can be differentiated preferably, molecular weight is close, the similar substance of structure and realizes instrument faster
Device cleans, then it is 0.6L/min to select migration pump discharge.
Fig. 7 is relaxed using the practical commercially available health products aloe constipation of UPLC-MS (ultra high efficiency liquid phase-mass spectrometry) method detection
The spectrogram that capsule obtains.(a) of Fig. 7 is the UPLC-MS spectrograms of phenolphthalein.(b) of Fig. 7 is the UPLC-MS spectrograms of caffeine.
Fig. 8-1 (a), Fig. 8-1 (b) are to detect practical city using ionic migration spectrometer using the method provided in embodiment
Sell spectrogram that is that health products aloe capsule for easying astriction obtains and being handled with Orgin8.6 softwares.Wherein horizontal axis is transit time
(millisecond), the longitudinal axis are the intensity (millivolt) of ion signal.It can be seen that instrument successfully detects the presence of synthetic drug ingredient,
It is consistent with the testing result of UPLC-MS in Fig. 7.Sample serial number see the table below shown in 2 in figure.
The serial number name of 2 Fig. 8-1 (a) of table
| Sample number | Sample ID | Holotype peak position (ms) | Negative mode peak position (ms) |
| 1# | Caffeine | 8.73ms±0.1 | |
| 2# | Hydrochloric acid-N-N- dinor- sibutramines | 11.45ms±0.1 | |
| 3# | Phenolphthalein | 11.23ms ± 0.1 (main peak) | 12.58ms±0.1 |
Fig. 9 is good for again clearly using the practical commercially available health products soup minister of UPLC-MS (ultra high efficiency liquid phase-mass spectrometry) method detection
The spectrogram that good clear smooth capsule obtains.
Figure 10-1 (a), Figure 10-1 (b) are to detect practical city using the method provided in embodiment ionic migration spectrometer
It sells health products soup minister and is good for spectrogram that is that clear good clear smooth capsule obtains and being handled with Orgin8.6 softwares again.Wherein horizontal axis is to move
Shift time (millisecond), the longitudinal axis are the intensity (millivolt) of ion signal.It can be seen that instrument confirmatory sample is free of synthetic drug ingredient,
It is consistent with the testing result of UPLC-MS in Fig. 9.
Instrumental results when following table 3 is for 210 DEG C of 120 kinds of slimming health food injector temperatures.By in table
Data show that edible substrates ingredient such as aloe, lotus leaf, cassia seed, rhizoma alismatis, lactose, the maltose in slimming health food can shadow
The detection for ringing experiment, causes instrument false alarm.
Table 3
It is taken for 46 kinds of samples before serial number and adjusts injector temperature to eliminate matrix interference problem, be specifically shown in Table 5.Table 4
For the detection limit of the common non-forensic chemistry Western medicine more added, as seen from the table, in 100 DEG C of injector temperature, instrument is to fiber crops
Yellow alkali, pseudoephedrine, sibutramine have good sensitivity, will not cause to fail to report it.Detection for caffeine, phenolphthalein
It then needs to carry out in 210 DEG C of injector temperature, is otherwise likely to cause and it is failed to report.
Table 4
Table 5
Therefore, postsearch screening method is used for part slimming health food, i.e.,：For in product contain aloe, lotus leaf,
Cassia seed, rhizoma alismatis, lactose, maltose health food, select injector temperature to avoid reporting by mistake for 100 DEG C of testing conditions screening
Afterwards, it then increases temperature, using the screening again of 210 DEG C of testing conditions, police is failed to report to avoid occur caffeine or phenolphthalein.Other
Slimming health food then need to only carry out under the testing conditions of 210 DEG C of injection port, include the health food to unknown packaging sample.
Testing conditions are respectively as shown in table 6, table 7.
The ionic migration spectrum detection condition of table 6, weight-reducing class standard product, health products：
Table 7 improves sleep class, hypoglycemic class, strengthen immunity/antifatigue class, adjusts blood pressure (blood fat) class standard product, protects
The ionic migration spectrum detection condition of health food：
As it can be seen that sensitive, quickly and efficiently can be detected to health products synthetic drug ingredient using the embodiment.
The 202 kinds of health foods sampled on the market using the detection method screening at present, are contained wherein announcing it in official
Have synthetic drug ingredient has 4 kinds, and contained synthetic drug is shown in Table 8.
Table 8, the health food testing result containing synthetic drug ingredient
24 kinds are selected from health food as laboratory sample, synthetic drug ingredient, additive capacity are added in artificial classification
Between 1~200mg/g.Gained testing result is shown in Table 9.As can be seen from the table, the testing result of IMS is detected with UPLC-MS
As a result and artificial addition situation is not much different.In table except No. 13 aloes just must relieving capsule using in addition to postsearch screening method, other 23
Kind sample is all made of primary screening method.
Table 9,24 kind of artificial health food testing result for adding synthetic drug ingredient
Claims (16)
1. the detection method of synthetic drug ingredient in a kind of food, which is characterized in that the method includes (1) to synthesis to be checked
The standard sample of drug ingedient is detected and establishes standard database respectively；(2) food samples are detected；(3) instrument from
It is dynamic that result is compared and drawn a conclusion with standard substance database；In step (2) the food samples ingredient containing aloe,
It is one or more in lotus leaf, cassia seed, rhizoma alismatis, lactose and maltose, it is described food samples to be detected to carry out twice
It detects to determine final analysis result, at 80-110 DEG C, second of injector temperature setting exists the setting of first time injector temperature
180-220 DEG C, the method is detected using ionic migration spectrometer.
2. detection method according to claim 1, which is characterized in that the input mode of the detection select direct sample into
Quadrat method.
3. detection method according to claim 2, which is characterized in that the direct sample feeding method includes to food sample
Product carry out unlap pre-treatment, by the wiping of treated food samples on sampling carrier and be inserted into the instrument of detection into
Sample mouth is detected.
4. detection method according to claim 1, which is characterized in that the method is detected using ionic migration spectrometer,
The testing conditions of ionic migration spectrometer include：Sampling line number is 40-100, sample introduction pump discharge 0-0.6L/min, migrates pump discharge
0.6-0.8L/min；The ion gate Voltage Pulse Width of ionic migration spectrometer is 300-800 μ s.
5. detection method according to claim 4, which is characterized in that the method is detected using ionic migration spectrometer,
The testing conditions of ionic migration spectrometer are：It is 50, sample introduction pump discharge 0L/min, migration pump discharge 0.6L/min to sample line number；From
The ion gate Voltage Pulse Width of sub- mobility spectrometer is 380 μ s.
6. detection method according to claim 4, which is characterized in that the testing conditions of the ionic migration spectrometer also wrap
It includes：Positive transfer tube temperature degree is set as 130-190 DEG C, and at 100-150 DEG C, injector temperature setting exists negative transfer pipe temperature setting
80-220℃。
7. detection method according to claim 6, which is characterized in that the testing conditions of the ionic migration spectrometer also wrap
It includes：Positive transfer tube temperature degree is set as 170 DEG C, and at 130 DEG C, injector temperature is arranged at 210 DEG C negative transfer pipe temperature setting.
8. detection method according to claim 4, which is characterized in that the clean conditions of ionic migration spectrometer include：Sample introduction
Blowback flow 0-0.6L/min is pumped, migration pump discharge is 0.6-0.8L/min.
9. detection method according to claim 8, which is characterized in that the clean conditions of ionic migration spectrometer are：Sampling pump
Blowback flow 0.6L/min, migration pump discharge are 0.6L/min.
10. detection method according to claim 8, which is characterized in that the clean conditions of ionic migration spectrometer further include：Just
Migration tube temperature setting is 130-190 DEG C, and at 100-150 DEG C, injector temperature is arranged in 80-220 negative transfer pipe temperature setting
DEG C, sample line number 40-100 items.
11. detection method according to claim 10, which is characterized in that the clean conditions of ionic migration spectrometer further include：
Positive transfer tube temperature degree is set as 170 DEG C, and at 130 DEG C, injector temperature is arranged at 210 DEG C negative transfer pipe temperature setting, samples line
Number 50.
12. according to the detection method described in claim 4~11 any one, which is characterized in that first time injector temperature is set
100 DEG C are set to, second of injector temperature is arranged at 210 DEG C.
13. according to the detection method described in claim 4~11 any one, which is characterized in that wherein step (1) includes：It will
The standard sample of synthetic drug ingredient to be checked is configured to the stock solution of 1mg/mL respectively, and is diluted to suitable concentration and is tested
Standard solution takes standard solution sample introduction, obtains the ion transfer spectrogram of standard sample, according to standard solution under various concentration
The ion transfer spectrogram of acquisition, the final characteristic peak for determining standard sample, i.e. transit time are respectively waited for by the type foundation of synthetic drug
Standard database of the synthetic drug of inspection about its feature transit time.
14. according to the detection method described in claim 1~11 any one, which is characterized in that the wherein described sample is health care
Food.
15. detection method according to claim 12, which is characterized in that the wherein described sample is health food.
16. detection method according to claim 13, which is characterized in that the wherein described sample is health food.
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| CN108061777B (en) * | 2017-11-27 | 2020-05-08 | 浙江公正检验中心有限公司 | Method for detecting residual quantity of 34 illegally added medicines in weight-losing health-care food |
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