CN103852498B - The quickly illegal method adding sibutramine in detection goods - Google Patents
The quickly illegal method adding sibutramine in detection goods Download PDFInfo
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- CN103852498B CN103852498B CN201210500344.XA CN201210500344A CN103852498B CN 103852498 B CN103852498 B CN 103852498B CN 201210500344 A CN201210500344 A CN 201210500344A CN 103852498 B CN103852498 B CN 103852498B
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Abstract
The present invention relates to quickly detect the method for illegal additive in fat-reducing quasi drugs, health product or food.Being specifically related to detection suspect mixed with the method whether containing sibutramine in the goods of sibutramine, the method comprises the following steps: it is appropriate that (1) takes described goods, mixes with special solvent, and shaking or ultrasonic wave added dissolve, and obtain mixing test solution；(2) suitable detectors based on the certain electric principles of chemistry are used to measure the certain electric chemical parameters of mixing test solution；(3) i.e. can determine whether whether goods may illegally be added with sibutramine according to the size of parameter value.The method of the present invention need not filtered sample solution, the most time-consuming 2 ~ 3 minutes of detection overall process, has the advantages such as quick, easy, safe, highly sensitive, environmental protection.
Description
Technical field
The present invention relates to the analysis technical field of a kind of medicine, health food or food, particularly relate to a kind of based on electrification
Learn the method for the illegal sibutramine added in rapid screening medicine, health food or the food of principle.
Background technology
Sibutramine (sibutramine) is that the Knoll company 5-in listing in 1997 is through tryptamines and norepinephrine
Its chemical entitled N-{1-of reuptake inhibitor [1-(4-chlorphenyl) cyclobutyl]-3-methyl butyl }-N, N'-dimethylamine, molecule
Structure exists a chiral carbon atom, it is possible to act on nervus centralis, accelerates metabolism and appetite-suppressing, the full sense of increase,
Promote internal energy expenditure, reduce blood lipid level and cholesterol levels, clinically for the treatment of obesity, there is absorption
Good, the feature such as determined curative effect.Sibutramine hydrochloride listing after, successively have about 10,000,000 people to use this product, sales volume also with
The annual rate of growth of 50% increases, and becomes and is popular in American-European best-selling slimming medicine.
U.S. food Drug Administration (US-FDA) in this medicine of official approval in November, 1997 as treatment obesity
Special-purpose medicaments, and specify to use under physician guidance.((SFDA) is in July, 2000 in Chinese food Drug Administration
After two kind new medicine approval listings, same regulation presses prescription drugs management.Under physician guidance, do not take sibutramine,
A series of untoward reaction and side effect can be produced, mainly have digestive system, cardiovascular system, neuropsychiatric bad instead
Should.It addition, take sibutramine also can produce some rare untoward reaction, mainly there are renal damage, the impact on sexual function, skin
Rash, alopecia etc..Clinician, when applying sibutramine, should be specifically noted that the observation to its untoward reaction, reduces to merge and uses
Medicine, forbids applying, to ensure the safety of medication person in elderly population teenage.
The adverse effect caused about sibutramine at present oneself have many reports, Britain, New Zealand, Italy etc. are many
Individual country report takes the people of sibutramine has untoward reaction, such as headache, giddy, dizzy, hypertension, tachycardia, cardiopalmus, breast
Bitterly, insomnia, anxiety-depression, Impairment of Memory and slight gastro-intestinal syndrome, in addition with the death report of many cases.China allows
Use sibutramine class fat-reducing medicine, but this type of medicine need be cautious use of, should use under physician guidance.During use, health is wanted
Monitoring at any time, should accept a series of inspections such as liver function, blood fat, albumen, blood pressure before using, the health in using also is wanted
Monitoring at any time just can ensure that safe medication.It disables in gestation, prepares gestation and women breast-feeding their children, and organic obesity is not (as having
The thyroid for the treatment of can be low) person, accept the patient that oxidase inhibitor (MAGI) is treated, the disease to sibutramine allergy
People, the patient of nervous anorexia, accept the patient of other central appetite suppressants.
But, the manufacturer of some fat-reducing quasi drugs and health product the most illegally mixes sibutramine.For having
Effect ground hit this false making mix puppet malpractice, ensure the people drug safety, necessary foundation reliably for
The illegal detection method mixing Western medicine Sibutramine hydrochloride.Western cloth song is added for illegal in fat-reducing quasi drugs and health food
Bright situation is on the rise, and country has carried out repeatedly focus efforts on special areas.National Drug Administration ratified on March 14th, 2006
Drug inspection for the Chinese patent medicine for the treatment of obesity supplements the method for inspection, approved document numbered 2006004.The method is suitable for
In the Chinese patent medicine for the treatment of obesity, it is accused of illegally adding the supervision and inspection of sibutramine, ephedrine, fenfluramine, uses
The western medicine composition added illegal in medicine is confirmed and assay by high performance liquid chromatography and liquid/matter combination method detection.
The instrument that the method relates to is much more expensive, and the consumptive material needed when using is not the most cheap, for substantial amounts of inspection, and extensively
This inspection activity is carried out in big rural area bigger difficulty.
At present, the detection method of sibutramine mainly has: thin layer chromatography, high performance liquid chromatography, high performance liquid chromatography
One MS etc., but these method apparatus expensive, operating cost are high, operating process complicated, are not suitable in basic unit
Department extensively carries out.Additionally, also utilize the quick differential method of chemical reaction, quickly differentiate that examination technology, with its low cost, is covered
The advantages such as capping is wide and obtained the attention of industry many personages.
Such as, Publication No. CN 101408519A (application number 200810028617.9, publication date on April 15th, 2009,
Invention entitled " a kind of method detecting Sibutramine hydrochloride and application thereof ") patent documentation disclose a kind of detection method:
(1) testing sample being firstly added ethyl acetate, jog makes to leach, and after standing, draws supernatant liquid;(2) to above-mentioned upper liquid
Adding extract phosphoric acid solution in body, jog makes two-phase mixtures, places layering, draws lower floor's solution;(3) by detection agent sulfur cyanogen
Whether the chromogenic reaction detection sample of ammonium chromate saturated solution exists Sibutramine hydrochloride.The operation of this method is relatively simple, but
Step is the most, and the effect obtained, from the beginning of preparation solution and developer, completes all operations the most time-consuming 10 minutes, and detection uses
The preparation of the saturated solution of sulfur cyanogen ammonium chromate needs to shake 1 hour, the most time-consuming, and is toxic reagent.
Electric conductivity detector can be used for measuring the electrical conductivity in solution.It is total that TDS water quality testing meter can be used for detecting in water
Dissolved solids (Total dissolved solids, TDS), with the degree of purity of evaluating water quality.Both detectors belong to fast
Speed Electrochemical Detection instrument, scholar it has been investigated that, it may be used for measuring the content of sodium chloride in sodium-chloride water solution.So
Whether directly can may add western cloth by the electrochemical method detection suspection of electrical conductivity or TDS in detection water bent
Bright fat-reducing quasi drugs, health product or food？Found that effect is unsatisfactory, this is because sibutramine may be added
Containing other hydroaropic substance in substrate complicated in fat-reducing quasi drugs, health product or food, meeting severe jamming sample solution
TDS (TDS) in electrical conductivity and solution, causes result and whether adds sibutramine and do not have dependency.The most straight
Connect with electrochemical method detection detection fat-reducing quasi drugs, health product or the food of electrical conductivity or TDS in detection solution
In the most illegally add sibutramine there is technical difficulty.
Therefore, people need nonetheless remain for that a kind of operation is simpler, speed faster and safer, pollute less capacity of resisting disturbance more
The strong method of inspection, in order to identify in medicine, health food and food whether add sibutramine quickly and accurately.
Summary of the invention
It is an object of the invention to provide one can quickly, detect suspection mixed with west easy, safety and/or low stain
The method whether containing sibutramine in the goods of cloth Qu Ming.The present inventor it has surprisingly been found that when use appropriate solvent time,
Use suitable Electrochemical detector or the electrochemical detection method can be the most at the scene to suspecting the system mixed with sibutramine
Product check, and method is quick, easy, safe and/or low stain.The present invention is accomplished based on above discovery.
To this end, first aspect present invention provides a kind of suspection that detects mixed with whether containing western cloth in the goods of sibutramine
The method of Qu Ming, the method comprises the following steps:
(1) take goods to be measured appropriate, mix with Extraction solvent that (thus, described Extraction solvent can provide proton, this matter
Son can associate with hydrogen bond mutually with sibutramine molecule), after shaking or ultrasonic wave added dissolve, obtain mixing test solution；
(2) the electrochemistry ginseng during electrochemical principle based on effects of ion displacement under the electric field measures mixing test solution
Number；
(3) judge that whether may add (the most unlawfully adding) in goods has sibutramine according to parameter size.
Any embodiment of the either side of the present invention, can be combined with other embodiment, as long as they are not
There will be contradiction.Additionally, in any embodiment of either side of the present invention, it is real that arbitrary technical characteristic goes for other
Execute this technical characteristic in scheme, as long as they do not have contradiction.
The invention will be further described below.
All documents recited in the present invention, their full content is incorporated herein by, and if these literary compositions
Offer expressed implication and the present invention inconsistent time, be as the criterion with the statement of the present invention.Additionally, the present invention use various terms and
Phrase has and well known to a person skilled in the art general sense, nonetheless, the present invention remain desirable at this these terms and
Phrase is described in more detail and explains, the term mentioned and phrase are if any inconsistent with common art-recognized meanings, with institute of the present invention table
The implication stated is as the criterion.
Terms used herein " mixes ", " mixed with ", " incorporation " etc., they can be intentionally or unintentionally to described goods
Middle addition sibutramine.
Method according to a first aspect of the present invention, wherein said goods, or described suspection is mixed with the goods of sibutramine,
It includes that aneroid any meaning gives any artificial manufactured goods of the mammal such as mankind, the most manually mixes system
Product, it includes being not limited to medicine, health food, food, food additive etc..In one embodiment, described goods are
Medicine, health food.Phrase " is suspected the goods mixed with sibutramine " and is referred to a kind of goods, and those skilled in the art are (particularly
Health/health/Yao Jian authorities or its staff) subjective or objectively think, these goods may be had a mind to or
Person is by mistake mixed with sibutramine, so that these goods can produce the life that sibutramine is had main or secondaryly
Thing effect, such as, produce the biological effect for the treatment of obesity.In the present invention, these goods are also referred to as sample, detection sample
Product etc., those skilled in the art refer to the implication that the different terms of these goods are had, such as according to the linguistic context understanding of the present invention
After making these goods shake with Extraction solvent, the mixing liquid obtained is properly termed as mixing test solution.In the present invention, these goods should be
Solid, such as powder or block or pellet or granular substance etc..
Method according to a first aspect of the present invention, described in step (1), Extraction solvent is proton solvent, the most organic molten
Agent.In one embodiment, described organic solvent includes but not limited to methanol, ethanol, ethyl acetate, acetone, dimethyl
Sulfoxide, dimethylformamide or a combination thereof, or their solution containing other materials.The effect of this Extraction solvent is to make west
The bent bright dissolving of cloth, and provide proton so that making sample solution have the electrochemical properties of suitably electrically conductive ability, extract molten in addition
Agent also has the effect preventing water solublity interfering material from dissolving and causing conductive capability to change.The most any it is capable of this function
Extract solution be all applicable.In one embodiment, described organic solvent is ethanol.The method according to the invention,
In step (1), described goods and the amount of Extraction solvent and ratio need not particularly limit, as long as goods and Extraction solvent mix
After conjunction, it is understood that there may be sibutramine dissolve in a solvent and reach the inventive method detection limit.Such as an enforcement
In scheme, the Extraction solvent in step (1) is 1 ~ 50ml, such as 5 ~ 20ml, such as 10 ~ 20ml；The amount of the goods taken is
0.1 ~ 10g, such as 0.5 ~ 5g.The method according to the invention, wherein in step (1) goods to be measured and Extraction solvent ratio be 0.5 ~
5g:10~20ml。
Method according to a first aspect of the present invention, the detector based on electrochemical principle of wherein said step (2) is electricity
Electrical conductivity instrument and/or TDS (i.e. TOTAL DISSOLVED SOLIDS) water quality testing meter.For implementing or easy to operate purpose,
The Electrochemical detector of the present invention can be miniature instrument or removable instrument or miniature lip pencil detector.Step (2) is surveyed
Fixed electrochemical parameter can be conductivity value and/or TDS value or other parameter relevant with above-mentioned electrochemical parameter.Such as exist
In one embodiment, conductivity meter is used to measure sample electrical conductivity in particular solution；In another embodiment, make
Sample TDS value in particular solution is measured with TDS water quality testing meter.
Method according to a first aspect of the present invention, wherein said step (3) is used for judging whether may contain west in goods
The parameter value of cloth Qu Ming is direct with the type of article usage to be measured, the type of Extraction solvent, the volume of Extraction solvent and parameter
Relevant.When article usage is a dose, and Extraction solvent is ethanol, the volume of step (2) Extraction solvent judges with step (3)
Goods whether may containing between the parameter value of sibutramine inversely, concrete numerical relation is: the volume of Extraction solvent
× parameter value electrical conductivity is about the volume × parameter TDS value of 320ml μ S/cm and/or Extraction solvent and is about 160ml ppm.
When article usage is a dose, and Extraction solvent is ethanol, and Extraction solvent volume is 20ml, location parameter is electricity
During conductance, it is judged that whether goods may the parameter value containing sibutramine be 16 μ S/cm, if the electrical conductivity of i.e. product solution
More than or equal to 16 μ S/cm, then can determine whether goods may contain sibutramine.
When article usage is a dose, and Extraction solvent volume is 10ml, and Extraction solvent is ethanol, location parameter is electricity
During conductance, it is judged that whether goods may the parameter value containing sibutramine be 32 μ S/cm, if the electrical conductivity of product solution is big
In equal to 32 μ S/cm, then can determine whether goods may contain sibutramine.
When article usage is a dose, and Extraction solvent volume is 20ml, and Extraction solvent is ethanol, and location parameter is
During TDS value, it is judged that whether goods may the parameter value containing sibutramine be 8ppm, if the TDS value of product solution is more than
Equal to 8ppm, then can determine whether goods may contain sibutramine.
When article usage is a dose, and Extraction solvent volume is 10ml, and Extraction solvent is ethanol, and location parameter is
During TDS value, it is judged that whether goods may the parameter value containing sibutramine be 16ppm, if the TDS value of product solution is more than
Equal to 16ppm, then can determine whether goods may contain sibutramine.
If described goods are judged as wherein may containing sibutramine, then these goods can use other method further
Detect, such as by the method for laboratory, such as HPLC method etc..So, method of the invention is particularly suitable in market
Upper or other detection scene carries out detection and the examination of more large sample, and and then the workload of minimizing laboratory.
Method based on first aspect present invention, second aspect present invention provides a kind of complete detection equipment, and it is used for
Detection is suspected mixed with whether containing sibutramine in the goods of sibutramine, and described complete detection equipment includes:
I () Extraction solvent, it is packaged in solvent bottle；
(ii) analyzer based on electrochemical principle；
(iii) operation instruction data, it records this complete detection equipment Inspection of use and suspects mixed with sibutramine
Whether goods contain the operational approach of sibutramine.
Complete detection equipment according to a second aspect of the present invention, described complete detection equipment is test kit.
Complete detection equipment according to a second aspect of the present invention, wherein said solvent bottle can repeatedly be opened and seal
Solvent bottle.The material of this solvent bottle is not particularly limited, such as, can be the vial with bottle stopper, bottle cap etc., plastic bottle etc..
In a preferred embodiment, the volume of the Extraction solvent loaded in described solvent bottle accounts for the 1/10 ~ 9/ of solvent bottle capacity
10, such as 3/10 ~ 8/10.In solvent bottle, reserved certain space is highly profitable, such as can be directly by straight for goods to be checked
Connect and join in solvent bottle, cover tightly, then shake, make goods to be checked be sufficiently mixed with Extraction solvent, to make possibility as much as possible
The sibutramine existed dissolves in the solution；The complete detection equipment that so present invention provides is the simplest.
Complete detection equipment according to a second aspect of the present invention, which includes more than one described in be packaged with extraction molten
The solvent bottle of agent.According to these embodiments, the invention provides and can detect multiple systems in same place or different location
The complete detection equipment of product material requested.
Complete detection equipment according to a second aspect of the present invention, which includes mensuration based on the certain electric principles of chemistry
Instrument, such as conductivity measuring instrument or TDS water quality testing meter.
Complete detection equipment according to a second aspect of the present invention, wherein said operation instruction data can be operation instruction
The explanation of book, detection method, detection criterion etc., its form can be to be printed with the paper of corresponding information, card etc., and this makes
The method described in first aspect present invention is substantially described with detail file.Therefore, the arbitrary embodiment party of first aspect present invention
In case, arbitrary technical characteristic therein is equally applicable to the complete detection equipment of second aspect present invention or is applicable to the present invention
Other side.
Third aspect present invention provides a kind of information detail file, the most substantially describes first aspect present invention and appoints
One described method.
In one embodiment, this information detail file is in selected from following form: paper document (includes but do not limits
In file single page, pamphlet, publication), magnetizing mediums, CD, floppy disk, electronic publication, Web publishing etc., and their group
Close.
Fourth aspect present invention provides information detail file detection according to a third aspect of the present invention and suspects mixed with western cloth bent
The method whether containing sibutramine in bright goods.
Fifth aspect present invention provides information detail file inspection according to a third aspect of the present invention and suspects mixed with western cloth bent
Bright goods.
It addition, step (1) gained mixing test solution is probably a kind of suspension in the inventive method, this mixing test solution need not
Filter and i.e. can be used for next step, which greatly simplifies operating procedure, be also particularly well-suited to the process of very small amount sample.
Therefore, in a preferred embodiment of the invention, it is provided that sibutramine in a kind of medicine, health food and food
Detection method, it comprises the steps:
(1) take solid-state medicine, health food or the food of a dose, add Extraction solvent ethanol 20ml, and shake or
Ultrasonic wave added dissolves 1 minute；
(2) without filtering, directly corresponding electrochemical parameter is measured with conductivity measuring instrument and/or TDS water quality testing meter.
(3) if electrical conductivity is more than or equal to 8ppm more than or equal to 16 μ S/cm and/or TDS value, then can determine whether can in sample
Can be containing sibutramine.
The present invention, compared with the method for quick of other sibutramine, has the advantage that
(1) result judges directly perceived: the result judgment mode of various methods is compared as follows.Compared with other patented method,
The present invention carries out result judgement according to objective detection numerical value, it is determined that mode is directly perceived, is not required to examine color variation tendency, is not subject to
The restriction of complex sample solution shades of colour and interference, be difficult to the situation occurring judging.
(2) quick: when using the present invention to detect, simple to operate, step is few, and whole process only needed less than 2 minutes
(sample dissolution needs 1 minute, and Instrument measuring and result judge to need 5 seconds).And time-consuming at least 5 ~ 10 minutes of other method.
(3) easy: compared with the method that other document is reported, the inventive method, without extraction, filtration, operates simpler
Just.
(4) detecting instrument is durable: compared with other patented methods, if carrying out hundreds of time detection, the present invention only needs to consume molten
Agent, instrument then need not be changed；Additive method then needs to consume matched hundreds of set chemistry identification reagents.
(5) safety and environmental protection: the present invention carries out using when differentiating to judge instrument detection, and other patented method then uses poisonous
Chromic thiocyanate ammonium salt solution.Therefore the inventive method more safety and environmental protection when differentiating to judge, to operator and environment without times
What impact.
(6) testing cost is low, it is simple to extensively application: compared with existing high performance liquid chromatography and liquid/matter combination method, detection
Equipment price and operating cost is relatively low, operating process is simple, it is adaptable to extensively carry out in department of basic unit.
Detailed description of the invention
The present invention is further illustrated below by concrete example, it should be understood, however, that, these examples are only used for
Specifically describe in more detail and be used, and be not to be construed as limiting in any form the present invention.
The present invention to test used in material and test method carry out generality and/or concrete description.Though
It is so to it is known in the art that still the present invention is still at this for realizing many materials that the object of the invention used and operational approach
Describe in detail as far as possible.It will be apparent to those skilled in the art that hereinafter, if not specified, material therefor of the present invention and
Operational approach is well known in the art.
Whether embodiment 1, detection medicine/health product contain the general operational requirement(GOR) of sibutramine
1, sampling amount:
Recommend sampling as follows in dissimilar sample:
| Sample type | Sampling amount |
| Tablet | One time oral dose (must grind) |
| Capsule | One time oral dose (takes content to grind) |
| Big honeyed pills | One time oral dose (must be pulverized) |
| Electuary | One time oral dose (must be pulverized) |
| Other solid | One time oral dose |
The amount of the product to be checked that the inventive method uses is few as can be seen here, in order to damage the profit of the operator of an innocent person as little as possible
Benefit, dose about 0.5 ~ 5g of the sample of any of the above type, such as capsule, tablet ampoule about 0.5g, and electuary,
Big honeyed pills ampoule reaches about 5g.
2, prepared by need testing solution
Get it filled product, health food or food, add ethanol 20ml, shake 1 minute.
3, colour developing judged result
Analyzer based on electrochemical principle is used to measure, when using TDS water quality testing meter to measure sample solution, if
TDS value is more than or equal to 8ppm, then can determine whether may illegally add in sample sibutramine, if TDS value is less than 8ppm,
Can determine whether in testing sample without sibutramine.The most if desired, to may gathering greater amount containing the sample of sibutramine,
Prepare to use other method such as chromatography to make further to judge.
Whether embodiment 2, detection medicine/health product contain the general operational requirement(GOR) of sibutramine
1, sampling amount:
Recommend sampling as follows in dissimilar sample:
| Sample type | Sampling amount |
| Tablet | One time oral dose (must grind) |
| Capsule | One time oral dose (takes content to grind) |
| Big honeyed pills | One time oral dose (must be pulverized) |
| Electuary | One time oral dose (must be pulverized) |
| Other solid | One time oral dose |
The amount of the product to be checked that the inventive method uses is few as can be seen here, in order to damage the profit of the operator of an innocent person as little as possible
Benefit.
2, prepared by need testing solution
Get it filled product, health food or food, add ethanol 20ml, shake 1 minute.
3, colour developing judged result
Analyzer based on electrochemical principle is used to measure, when using electric conductivity detector to measure sample solution, if electric
Conductivity value is more than or equal to 16 μ S/cm, then can determine whether may illegally add in sample sibutramine, if conductivity value is less than
16 μ S/cm, then can determine whether in testing sample without sibutramine.The most if desired, can to the sample that may contain sibutramine
Gather greater amount, prepare to use other method such as chromatography to make further and judge.
Whether embodiment 3, detection medicine, health food and food exist the test of sibutramine
The method using embodiment 1 quickly detects 20 batch samples (being Yao Jian department examination at random sample).Further according to " country
Drug and food Surveillance Authority drug inspection supplements the method for inspection and inspection project approval part 2006004 ", use HPLC/MS/MS
Method detection sample, to verify screening results.
Drug inspection supplements the detection method of the HPLC/MS/MS of the method for inspection and inspection project approval part 2006004 record
As follows:
Chromatographic condition: mobile phase A is 0.02mol/L ammonium acetate, Mobile phase B is 0.1% acetic acid aqueous solution/acetonitrile, by following
Gradient table carries out eluting.
| Time (min) | A(%) | B(%) |
| 0.00 | 70 | 30 |
| 12.00 | 70 | 30 |
| 18.00 | 50 | 50 |
| 25.00 | 50 | 50 |
| 35.10 | 10 | 90 |
| 40.00 | 10 | 90 |
Mass Spectrometry Conditions: ESI source, source voltage 5kV, capillary temperature 275 DEG C, capillary voltage 15V, sheath gas velocity 40arb,
Cation detects, full scan first mass spectrometric, full scan second order ms, sweep limits m/z:100 ~ 1000.
According to the form below, takes the various solid samples of one time oral dose, adds ethanol 20ml, shakes 1 minute.Then use based on electricity
The analyzer of the principles of chemistry measures.When using TDS water quality testing meter to measure sample solution, if TDS value is more than or equal to 8ppm, then
Can determine whether sample may illegally add sibutramine, if TDS value is less than 8ppm, can determine whether testing sample does not contains
Sibutramine；When using conductivity meter to measure sample solution, if conductivity value is more than or equal to 16 μ S/cm, then can determine whether tested
Sample may illegally add sibutramine, if conductivity value is less than 16 μ S/cm, then can determine whether in testing sample without western cloth
Qu Ming.
Result is as follows:
#: each goods be the different production firms that obtain of pharmacy from the market or health product shop and/or different size and/
Or the goods of different batches, suspect and be likely to be of the biological action being similar to sibutramine.
Above-mentioned experimental result shows with LC-MS HPLC/MS/MS assay, none official holiday sun of detection method
Property report, the simultaneously any sample containing sibutramine of the most non-missing inspection, result is accurately and reliably.
Sampling as described by this patent method measures 12 samples that the detection of above-mentioned sibutramine is negative, and divides
Not Can Ru sibutramine reference substance 5mg, test by the inventive method, result is all positive, and shows that this method has good
Good capacity of resisting disturbance, specificity is strong, has good accuracy.
Although it addition, above when testing 20 samples the inventive method with have beat all one with mass spectrometry method
The result caused, but inventor is when using methanol to substitute ethanol as reagent, has two kinds of method test results of some samples
Inconsistent, such as when being Extraction solvent test sample 3,6,13,15 etc. with methanol, result that the inventive method is judged and mass spectrum
Result is inconsistent.It addition, when using 5ml or 30ml to extract in above sample, have 8 samples and 11 samples to be judged respectively
Result inconsistent with mass spectral results；Result and the mass spectrum that 7 samples are judged additionally is had when the solvent used is 90% ethanol
Result is inconsistent.
Embodiment 3, the performance of the inventive method
The present embodiment investigates inventive method to sibutramine reference substance and the detection limit of sample, specific as follows:
Take the sibutramine reference substance 10.5mg that National Institute for Food and Drugs Control provides, add ethanol 20ml and dissolve preparation
Become the solution respectively containing 0.525mg sibutramine in every 1ml.Then analyzer based on electrochemical principle is used to measure.Result is such as
Shown in following table:
According to above-mentioned experimental result, can determine whether that the sensitivity of the inventive method detection sibutramine can reach to detect list
The effect of the sibutramine of minimum gauge in the preparation of position.
Take sibutramine reference substance 5.3mg and 10mg that National Institute for Food and Drugs Control provides, add ethanol respectively
20ml dissolves the solution being configured in every 1ml respectively to contain 0.265mg and 0.5mg sibutramine.Then use based on electrochemical principle
Analyzer measure.Result is as shown in the table:
According to above-mentioned experimental result, can determine whether that the sensitivity of the inventive method detection sibutramine at least can reach clinical single
The 53% of secondary consumption.
The present invention is by being described in detail the most to various aspects of the present invention, but the present invention is not limited to described
These specific embodiments, the spirit and scope of the present invention should be as the criterion with appended claims.The method of the present invention need not
Filtered sample solution, the most time-consuming 2 ~ 3 minutes of detection overall process, there is quick, easy, safety, sensitivity advantages of higher.
Claims (8)
1. the method for sibutramine in detection goods, the method comprises the following steps:
(1) taking goods to be measured appropriate, mix with Extraction solvent, described Extraction solvent provides proton and sibutramine molecule with hydrogen
Key associates mutually, after shaking or ultrasonic wave added dissolve, obtains mixing test solution；Described Extraction solvent is ethanol；
(2) electrochemical parameter during electrochemical principle based on effects of ion displacement under the electric field measures mixing test solution,
Described electrochemical parameter is electrical conductivity and/or TDS value；
(3) judge whether goods may illegally be added with sibutramine according to parameter size.
Method the most according to claim 1, wherein the detection equipment of step (2) described electrochemical principle be conductivity meter and/or
TDS water quality testing meter.
Method the most according to claim 1, wherein in step (1) goods to be measured and Extraction solvent ratio be 0.5～5g:10～
20ml。
4. a complete detection equipment, it is for detecting whether suspection contains sibutramine mixed with in the goods of sibutramine, its
Being characterised by, described complete detection equipment includes:
I () Extraction solvent, it is packaged in solvent bottle；Described Extraction solvent is ethanol；
(ii) analyzer based on electrochemical principle；The analyzer of described electrochemical principle is conductivity measuring instrument and/or TDS water
Quality detection instrument；
(iii) operation instruction data, it describes the method described in any one of claim 1-3.
Complete detection equipment the most according to claim 4, described complete detection equipment include more than one described in be packaged with and carry
Take the solvent bottle of solvent.
Complete detection equipment the most according to claim 4, described solvent bottle is the solvent bottle can repeatedly opened and seal.
Complete detection equipment the most according to claim 4, described solvent bottle is vial.
Complete detection equipment the most according to claim 4, the volume of the Extraction solvent loaded in described solvent bottle accounts for solvent bottle to be held
The 1/10～9/10 of amount.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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