CN106770765B - The detection method and application of a kind of albendazole and its metabolin - Google Patents
The detection method and application of a kind of albendazole and its metabolin Download PDFInfo
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Abstract
The invention discloses the detection methods of a kind of detection albendazole and its metabolin, belong to drug measurement techniques field.The detection method of the albendazole and its metabolin is the albendazole and its metabolin extracted in sample using 2,6-di-tert-butyl p-cresol and NaOH, is detected later using high performance liquid chromatography mass spectrometer；The concentration of the 2,6-di-tert-butyl p-cresol is 1%；The concentration of the NaOH solution is 50%.The beneficial effects of the present invention are: this method is not only applicable to animal muscle, the detection of the complex matrices such as liver is applied also for, reagent toxicity used in the present invention is small, and it is at low cost, save the time, moreover it is possible to efficiently reduce the extraction to impurity, simplify purifying step；It is detected using high performance liquid chromatography-tandem mass method, compared to single high performance liquid chromatography, there is high sensitivity, reproducible, detection limits low advantage.
Description
Technical field
The invention belongs to drug measurement techniques fields, and in particular to the detection method of a kind of albendazole and its metabolin and
Using.
Background technique
Currently, using big solvents of toxicity such as ether, acetonitriles in the method for detection albendazole, or directly use acetonitrile
It extracts, these methods not only make sample extraction insufficient, but also target compound is easily destroyed during the extraction process, thus
Influence quantitative result.
Summary of the invention
In order to solve the problems in the prior art, the technical solution adopted by the present invention is that:
The detection method of a kind of albendazole and its metabolin utilizes 2,6-di-tert-butyl p-cresol and NaOH to extract sample
In albendazole and its metabolin, detected later using high performance liquid chromatography mass spectrometer；2, the 6- di-t-butyl pair
The concentration of cresols is 1%；The concentration of the NaOH solution is 50%.
On the basis of above scheme, steps are as follows for the detection method of the albendazole and its metabolin:
1) extraction purification
Sample 5.00g is weighed, 5mL water, 150 μ L 50%NaOH solution and 1mL 1%2 is added, 6- di-t-butyl is to first
Phenol, vortex mixed add 20mL ethyl acetate, vibrate 1min ultrasonic extraction 20min, and 4000r/min is centrifuged 5min, takes supernatant
10mL ethyl acetate is added into residue and repeats to extract once for liquid, and supernatant is in pear shape bottle twice for merging, and 40 DEG C of revolvings are extremely
It is dry；6mL acetonitrile is added into the pear shape bottle after being spin-dried for and is saturated n-hexane, oscillation is mixed, poured into centrifuge tube, then into pear shape bottle
2mL acetonitrile is added, is poured into centrifuge tube together after the ultrasound 1min that is vortexed, the hydrochloric acid that 6mL 0.1mol/L is added into centrifuge tube is molten
Liquid, vortex 2min, 4000r/min are centrifuged 5min, remove n-hexane layer, spare；If emulsification, ultrasound and after being stirred with suction pipe from
The heart；
2) column purification is purified
After 5mL methanol and 5mL water balance activation PCX solid-phase extraction column, takes extracting solution to cross PCX decontaminating column, use 3mL respectively
Then water and the elution of 3mL methanol are the elution of 5% ammonium hydroxide methanol solution with 15mL volumetric concentration, received eluent is revolved in 40 DEG C
It steams to after doing；It is separately added into 1mL methanol and 1mL water, is vortexed, 0.22 μm of nylon leaching film is crossed, it is to be measured；
3) high performance liquid chromatography mass spectrometer detects
Mass spectrometry parameters: the source ion source AJS ESI；Gas Temp:325 DEG C；Gas Flow:10L/min；Sheath Gas
Temp350℃；Sheath Gas flow:11L/min；
Liquid phase parameter: A is 0.1% aqueous formic acid, and B is methanol.
On the basis of above scheme, the detection method of the albendazole and its metabolin is applied to detect animal derived
Albendazole and its metabolin in food.
On the basis of above scheme, the animal derived food is muscle, eggs, newborn class, liver and kidney.
Beneficial effects of the present invention:
Extract albendazole and its metabolin with 2,6-di-tert-butyl p-cresol and NaOH in the method for the present invention, toxicity compared with
It is small；In addition, albendazole and its metabolin be in aqueous solution alkalinity, be added mass concentration be 50%NaOH aqueous solution can make Ah
Parbendazole and its metabolin are conducive to organic reagent and extract at molecular state；It is 1%2,6- di-t-butyl to first that mass concentration, which is added,
It is not oxidized that phenol can protect albendazole；Ethyl acetate is the organic reagent of low pole, and addition is conducive to albendazole
It extracts and what impurity extracted lacks；Acetonitrile saturation n-hexane is used to remove the grease type impurity in sample, and hydrochloric acid, which is added, can make acetysalicylic acid phenobarbital
Be conducive to PCX purification column purification at ionic condition up to azoles；5% ammonium hydroxide methanol is in strong basicity, and when elution can adsorb PCX decontaminating column
Albendazole replace.
Method detection range of the invention is wider, and compared to the single-matrix of other methods, this method is not only applicable to
Animal muscle and the detection for being also applied for the complex matrices such as liver, it is well known that animal's liver contain many albumen, fat,
Carbohydrate, vitamin and mineral, purification completely do not influence target compound recycling very big；Method of the invention uses 2,6- bis-
As extracting solution, small toxicity is at low cost for Butylated Hydroxytoluene, NaOH and ethyl acetate, saves the time, and can efficiently reduce pair
The extraction of impurity simplifies purifying step；This method uses Agilent PCX solid phase extraction column, it is also possible to domestic PCX pillar generation
It replaces, testing cost is effectively reduced；It is detected using high performance liquid chromatography-tandem mass method, compared to single efficient liquid phase
Chromatography has high sensitivity, and reproducible, detection limits low advantage.
Detailed description of the invention
The measurement of Fig. 1 albendazole -2- amino sulfone retention time, wherein ordinate is response, and abscissa is retention time.
Fig. 2 albendazole -2- amino sulfone quantitative and qualitative ion detail, wherein ordinate is response, and abscissa is when retaining
Between.
Fig. 3 albendazole -2- amino sulfone mass spectrogram, wherein ordinate is response, abscissa m/z.
The measurement of Fig. 4 albendazole-sulfoxide retention time, wherein ordinate is response, and abscissa is retention time.
Fig. 5 albendazole-sulfoxide quantitative and qualitative ion detail, wherein ordinate is response, and abscissa is retention time.
Fig. 6 albendazole-sulfoxide mass spectrogram, wherein ordinate is response, abscissa m/z.
The measurement of Fig. 7 Albendazole sulfone retention time, wherein ordinate is response, and abscissa is retention time.
Fig. 8 Albendazole sulfone quantitative and qualitative ion detail, wherein ordinate is response, and abscissa is retention time.
Fig. 9 Albendazole sulfone mass spectrogram, wherein ordinate is response, abscissa m/z.
The measurement of Figure 10 albendazole retention time, wherein ordinate is response, and abscissa is retention time.
Figure 11 albendazole quantitative and qualitative ion detail, wherein ordinate is response, and abscissa is retention time.
Figure 12 albendazole mass spectrogram, wherein ordinate is response, abscissa m/z.
The standard curve of Figure 13 albendazole -2- amino sulfone, wherein ordinate is peak area response, and abscissa reaches for acetysalicylic acid phenobarbital
Azoles -2- amino sulfone concentration.
The standard curve of Figure 14 albendazole-sulfoxide, wherein ordinate is peak area response, and abscissa is that albendazole is sub-
Sulfone concentration.
The standard curve of Figure 15 Albendazole sulfone, wherein ordinate is peak area response, and abscissa is that Albendazole sulfone is dense
Degree.
The standard curve of Figure 16 albendazole, wherein ordinate is peak area response, and abscissa is albendazole concentration.
Figure 17 albendazole and its metabolin quota ion S/N figure, wherein ordinate is response, and abscissa is when retaining
Between, it is followed successively by albendazole -2- amino sulfone, albendazole-sulfoxide, Albendazole sulfone, albendazole from top to bottom.
Specific embodiment
Term as used in the present invention generally has those of ordinary skill in the art usual unless otherwise specified
The meaning of understanding.
Combined with specific embodiments below, and referring to the data further detailed description present invention.Following embodiment only be
It illustrates the present invention, rather than limits the scope of the invention in any way.
Embodiment
1. the preparation of standard solution
The preparation of 1.1 stock solutions
10.00mg albendazole, albendazole -2- amino sulfone, albendazole-sulfoxide and Albendazole sulfone are weighed respectively
Standard items are dissolved into methanol, constant volume to 10mL, the stock solution (be placed in -18 DEG C stored refrigerated) as 1000mg/L.
The preparation of 1.2 standard intermediate fluids
It is accurate respectively to measure 1mL albendazole, albendazole -2- amino sulfone, albendazole-sulfoxide and Albendazole sulfone mark
The stock solution of quasi- product, is dissolved into methanol, constant volume to 10mL, and the standard intermediate fluid as 100mg/L (is placed in -18 DEG C of refrigerations to protect
It deposits).
The preparation of 1.3 standard working curves
The standard liquid for being configured to 1,5,10,20,50,100 μ g/L with standard intermediate fluid is (fixed with methanol+water (v/v=1:1)
Hold), the standard solution as working curve.
2. sample treatment
2.1 extraction purification
Sample 5.00g is weighed, 5mL water, 150 μ L 50%NaOH solution and 1mL 1%2 is added, 6- di-t-butyl is to first
Phenol, vortex mixed add 20mL ethyl acetate, vibrate 1min ultrasonic extraction 20min, and 4000r/min is centrifuged 5min, takes supernatant
10mL ethyl acetate is added into residue and repeats to extract once for liquid, and supernatant is in pear shape bottle twice for merging, and 40 DEG C of revolvings are extremely
It is dry；6mL acetonitrile is added into the pear shape bottle after being spin-dried for and is saturated n-hexane, oscillation is mixed, poured into centrifuge tube, then into pear shape bottle
2mL acetonitrile is added, is poured into centrifuge tube together after the ultrasound 1min that is vortexed, the hydrochloric acid that 6mL 0.1mol/L is added into centrifuge tube is molten
Liquid, vortex 2min, 4000r/min are centrifuged 5min, remove n-hexane layer, spare；If emulsification, ultrasound and after being stirred with suction pipe from
The heart；
2.2 purification column purifications
After 5mL methanol and 5mL water balance activation PCX solid-phase extraction column, takes extracting solution to cross PCX decontaminating column, use 3mL respectively
Then water and the elution of 3mL methanol are the elution of 5% ammonium hydroxide methanol solution with 15mL volumetric concentration, received eluent is revolved in 40 DEG C
It steams to after doing；It is separately added into 1mL methanol and 1mL water, is vortexed, 0.22 μm of nylon leaching film is crossed, it is to be measured；
3. high performance liquid chromatography mass spectrometer detects
The high performance liquid chromatography mass spectrometer used is Agilent LC-MSMS 1290/6460；
Mass spectrometry parameters: the source ion source AJS ESI；Gas Temp:325 DEG C；Gas Flow:10L/min；Sheath Gas
Temp350℃；Sheath Gas flow:11L/min.
Liquid phase parameter: A is 0.1% aqueous formic acid, and B is methanol.Eluent gradient is as shown in table 1:
1 eluent gradient of table
| Time | Methanol concentration |
| 1.00 | 20 |
| 2.00 | 100 |
| 4.00 | 100 |
| 4.01 | 20 |
| 5.5 | 20 |
4. result and analysis
4.1 mass spectral results
The mass spectral results of albendazole and its metabolin are as shown in table 2:
2 mass spectral results of table
4.2 specificity
4.2.1 the specificity of albendazole -2- amino sulfone
50ppb albendazole -2- amino sulfone determines retention time by C18 chromatography post separation.As shown in Figure 1, when retaining
Between about 2.4min, and the peak shape of chromatography is preferable, and noiseless peak occurs, and wherein abscissa is retention time, and ordinate is response.
As shown in Fig. 2, wherein ordinate is response, abscissa is albendazole -2- amino sulfone quantitative and qualitative ion detail
Retention time.
As shown in figure 3, machine on 1ppm albendazole -2- amino sulfone, optimizes to obtain 3 ion pairs, ordinate by mass spectrum
For response, abscissa m/z.
4.2.2 the specificity of albendazole-sulfoxide
50ppb albendazole-sulfoxide determines retention time by C18 chromatography post separation.As shown in figure 4, retention time is about
For 2.9min, and the peak shape of chromatography is preferable, and noiseless peak occurs, and wherein abscissa is retention time, and ordinate is response.
For albendazole-sulfoxide quantitative and qualitative ion detail as shown in figure 5, wherein ordinate is response, abscissa is when retaining
Between.
As shown in fig. 6, machine on 1ppm albendazole-sulfoxide, optimizes to obtain 3 ion pairs by mass spectrum, ordinate is to ring
It answers, abscissa m/z.
4.2.3 the specificity of Albendazole sulfone
50ppb Albendazole sulfone determines retention time by C18 chromatography post separation.As shown in fig. 7, retention time is about
2.9min, and the peak shape of chromatography is preferable, noiseless peak occurs.Wherein abscissa is retention time, and ordinate is response.
For Albendazole sulfone quantitative and qualitative ion detail as shown in figure 8, wherein ordinate is response, abscissa is when retaining
Between.
As shown in figure 9, machine on 1ppm Albendazole sulfone, optimizes to obtain 3 ion pairs by mass spectrum, ordinate is response,
Abscissa is m/z.
4.2.4 the specificity of albendazole
50ppb Albendazole sulfone determines retention time by C18 chromatography post separation.As shown in Figure 10, retention time is about
3.159min, and the peak shape of chromatography is preferable, noiseless peak occurs, and abscissa is retention time, and ordinate is response.
Albendazole quantitative and qualitative ion detail is as shown in figure 11, and wherein ordinate is response, and abscissa is retention time.
As shown in figure 12, machine on 1ppm albendazole respectively obtains 3 ion pairs by mass spectrum optimization, and ordinate is response,
Abscissa is m/z.
4.3 standard curve
4.3.1 the standard curve of albendazole -2- amino sulfone
Precision draws albendazole -2- amino sulfone standard items, and being diluted to series of concentrations with 50% methanol aqueous solution is 1,5,
10,20,50,100ng/mL standard solution, sample introduction measurement respectively, using peak area response as ordinate, albendazole -2- amino sulfone
Concentration is abscissa.As shown in figure 13, the regression equation for obtaining albendazole -2- amino sulfone is Y=1378.144404*X-
594.187990, R2=0.9999, by related coefficient as it can be seen that in 1ng/mL~100ng/mL standard curve range of linearity,
UPLC-MSMS method measurement linear relationship is good, this standard curve can be used for accurate quantitative analysis.
4.3.2 the standard curve of albendazole-sulfoxide
Precision draws albendazole-sulfoxide standard items, and being diluted to series of concentrations with 50% methanol aqueous solution is 1,5,10,20,
50,100ng/mL standard solution, sample introduction measurement respectively, using peak area response as ordinate, albendazole-sulfoxide concentration is horizontal seat
Mark.As shown in figure 14, the regression equation for obtaining albendazole-sulfoxide is Y=519.827117*X-28.361658, R2=
0.9998, by related coefficient as it can be seen that in 1ng/mL~100ng/mL standard curve range of linearity, UPLC-MSMS method measures line
Sexual intercourse is good, this standard curve can be used for accurate quantitative analysis.
4.3.3 the standard curve of Albendazole sulfone
Precision draws Albendazole sulfone standard items, and being diluted to series of concentrations with 50% methanol aqueous solution is 1,5,10,20,
50,100ng/mL standard solution, sample introduction measurement respectively, using peak area response as ordinate, Albendazole sulfone concentration is abscissa.
As shown in figure 15, the regression equation for obtaining Albendazole sulfone is Y=1384.923769*X-533.206880, R2=0.9998,
By related coefficient as it can be seen that in 1ng/mL~100ng/mL standard curve range of linearity, it is good that UPLC-MSMS method measures linear relationship
Good, this standard curve can be used for accurate quantitative analysis.
4.3.4 albendazole
Precision draws albendazole standard items, and being diluted to series of concentrations with 50% methanol aqueous solution is 1,5,10,20,50,
100ng/mL standard solution, sample introduction measurement respectively, using peak area response as ordinate, albendazole concentration is abscissa.Such as figure
Shown in 16, the regression equation for obtaining albendazole is Y=8382.358953*X-2437.446609, R2=0.9999, by correlation
For coefficient as it can be seen that in 1ng/mL~100ng/mL standard curve range of linearity, UPLC-MSMS method measurement linear relationship is good, this
Standard curve can be used for accurate quantitative analysis.
4.4 detection limit
Addition is equivalent to sample and contains the albendazole of 1.0 μ g/kg and its standard items of metabolin in matrix, premenstrual to locate
Machine testing in reason calculates its signal-to-noise ratio (S/N) > 10, as shown in figure 17.
It measures the method for the present invention and 1.0 μ g/kg is limited to the detection of albendazole and its metabolin.
4.5 verifying matrixes and the rate of recovery
The verifying of matrix and the rate of recovery is as shown in table 3:
The verifying of 3 matrix of table and the rate of recovery
Commercially beef, pork liver, pig kidney, from supermarket's purchase egg, raw milk, crucian matrix do mark-on and test back
Between yield 70%-90%, illustrate that this method has good stability.
5. conclusion
By with UPLC-LCMSMS method in animal sources matrix albendazole and its metabolin be measured, determine
It is extracted using 2,6-di-tert-butyl p-cresol, NaOH and ethyl acetate, n-hexane purifying, PCX pillar is purified, and Ah is made
Parbendazole and its metabolin chromatographic peak reach baseline separation, and peak shape is good, and detection limits low, high sensitivity, and method recycling is stablized, this
Research is that the measurement of the albendazole and its metabolite residue amount in animal sources matrix establishes a kind of reliably analysis method.
Claims (3)
1. the detection method of a kind of albendazole and its metabolin, it is characterised in that: steps are as follows:
1) extraction purification
Sample 5.00g is weighed, 5mL water, 150 μ L 50%NaOH solution and 1mL 1%2,6- di-tert-butyl p-cresol, whirlpool is added
Rotation mixing, adds 20mL ethyl acetate, vibrates 1min ultrasonic extraction 20min, and 4000r/min is centrifuged 5min, takes supernatant, to
Addition 10mL ethyl acetate repeats to extract primary in residue, and merging supernatant twice, in pear shape bottle, 40 DEG C are rotated to dry；Xiang Xuan
6mL acetonitrile is added in pear shape bottle after dry and is saturated n-hexane, oscillation is mixed, poured into centrifuge tube, then 2mL is added into pear shape bottle
Acetonitrile, be vortexed ultrasound 1min after pour into centrifuge tube together, into centrifuge tube be added 6mL 0.1mol/L hydrochloric acid solution, vortex
2min, 4000r/min are centrifuged 5min, remove n-hexane layer, spare；If emulsification, ultrasound is simultaneously centrifuged after being stirred with suction pipe；
2) column purification is purified
After 5mL methanol and 5mL water balance activation PCX solid-phase extraction column, extracting solution is taken to cross PCX decontaminating column, respectively with 3mL water and
Then the elution of 3mL methanol is the elution of 5% ammonium hydroxide methanol solution with 15mL volumetric concentration, received eluent rotates extremely in 40 DEG C
After dry；It is separately added into 1mL methanol and 1mL water, is vortexed, 0.22 μm of nylon leaching film is crossed, it is to be measured；
3) high performance liquid chromatography mass spectrometer detects
Mass spectrometry parameters: the source ion source AJS ESI；Gas Temp:325 DEG C；Gas Flow:10L/min；Sheath Gas
Temp350℃；Sheath Gas flow:11L/min；
Liquid phase parameter: A is 0.1% aqueous formic acid, and B is methanol.
2. the application of albendazole and its metabolism object detecting method according to claim 1, it is characterised in that: dynamic for detecting
Albendazole and its metabolin in object derived food.
3. the application of albendazole and its metabolism object detecting method according to claim 2, it is characterised in that: the animal sources
Property food be muscle, eggs, newborn class, liver and kidney.
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