CN107290468B - A kind of method of betel nut alkali content in LC-MS quantitative detection children's indigestion tablet - Google Patents
A kind of method of betel nut alkali content in LC-MS quantitative detection children's indigestion tablet Download PDFInfo
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Abstract
The invention discloses a kind of methods of betel nut alkali content in LC-MS quantitative detection children's indigestion tablet.In the liquid chromatogram, mobile phase is made of methanol and 10mmol/l ammonium acetate solution, using gradient elution.The mass spectrum uses electron spray positive ion source, multiple-reaction monitoring analytical model (MRM)；Arecaline linear relationship within the scope of 50~2000ng/ml is good in this method.Test solution pre-treating method is easy to operate compared with HPLC method, and the operating time is short, and detection method specificity is strong, high sensitivity, analysis time are short, can be used for assay, the control of helping digestion of baby tablet quality of arecaline.
Description
Technical field
The invention belongs to Pharmaceutical Analysis fields, and in particular to arecaline in a kind of LC-MS quantitative detection children's indigestion tablet
The method of content.
Background technique
Children's indigestion tablet is recorded in the Pharmacopoeia of the People's Republic of China 2015 version one, and this product is the piece of light brown；Or
For special-shaped Film coated tablets.Multistep work is passed through by Endothelium Corneum Gigeriae Galli (parched), hawthorn, Medicated Leaven (stir-fry), coloured malt, betel nut, dried orange peel Six-element Chinese medicine
Skill is made.Major function is relieving dyspepsia, strengthening the spleen and stomach.For stagnant symptoms include deficiency of food caused by food stagnation stomach, constipation, stomach duct and abdomen is swollen
It is full, lean and haggard.The medicine entrance sweet and sour taste, has the advantages that be easy to receive children.Clinically for treating digestant for baby
Class disease is the standing drug of family.Pharmacology physiological activity of the arecaline in children's indigestion tablet is mainly manifested in the sympathetic mind of stimulation
Passed through extracellular Ca2+Interior stream mediate excited M choline receptor, make gastrointestinal smooth Muscle tensility increase, enhance enterocinesia, increase
Add digestive juice secretion, increase appetite, plays the role of helping digestion.But excessive arecaline can cause toxicity.Arecaline at present
The measuring method of content mainly has acid-base titration, thin layer chromatography scanning, capillary electrophoresis, high performance liquid chromatography (HPLC) method
Deng.Due to children's indigestion tablet complicated component, acid-base titration can only measure the content of total alkaloid；Thin layer chromatography scanning, capillary
Electrophoresis operation is complicated, accuracy is low；HPLC method accuracy height but sample pre-treatments complex steps, time-consuming, method sensitivity
It is lower.Therefore these methods all have some limitations.
Summary of the invention
In order to overcome defect and deficiency of the existing technology, the present invention provides a kind of favorable reproducibility, high sensitivity, divide
The method that analysis speed is fast, sample pre-treatments simply detect betel nut alkali content in children's indigestion tablet, this method can be used for arecaline
Assay, the control of helping digestion of baby tablet quality, beneficial reference is provided to production process and drug safety.
A kind of method of betel nut alkali content in LC-MS quantitative detection children's indigestion tablet, including step (1) sample preparation,
(2) prepared by standard curve, and (3) detect betel nut alkali content using liquid chromatograph mass spectrography.
(1) takes about 0.6g if the step of sample preparation includes: to take this product dry plate after finely ground, accurately weighed, sets 25ml
In measuring bottle, 0.9% sodium chloride injection is added to be settled to scale, sets on magnetic stirring apparatus with 850r/min revolving speed, stir 5min.I.e.
Obtaining concentration is 24mg/ml test sample suspension.
Precision pipettes test sample suspension 3ml, sets in EP pipe, after ultrasonic 30min, 0.22 μm of MICRO PES polyether sulfone water
Mesentery filtering, precision measure 500 μ l of subsequent filtrate, 10 μ l of 490 μ l of methanol and internal standard stock solution, set in EP pipe, mix, as examination
Product sample introduction solution.
Diazepam is designated as in the internal standard stock solution.
The step of prepared by (2) standard curve, which includes: that difference is accurate, measures Arecoline hydrobromide reference substance stock solution 5,
20,50,100,200 μ l, 10 μ l of internal standard stock solution, appropriate diluent are 1000 μ l to final volume, calibration curve solution are made,
Using the method detection of (3) liquid chromatograph mass spectrography detection, the corresponding peak face of Arecoline hydrobromide of each concentration is recorded
Product；Using Arecoline hydrobromide and interior target peak area ratio as ordinate, using the concentration of Arecoline hydrobromide as abscissa X, system
The equation of linear regression of standby Arecoline hydrobromide.
The step (3) using liquid chromatograph mass spectrography detect the step of include:
(a) liquid phase chromatogram condition chromatographic column: C18 column；Mobile phase: A:10mmol/l ammonium acetate solution is (extremely with formic acid tune pH
5.2)；B: methanol.Type of elution: gradient elution；Gradient program is as follows: 0~0.5min, 15% (v/v) B；2.1~
3.0min, 90% (v/v) B；3.1~6min, 15% (v/v) B.
(b) Mass Spectrometry Conditions mass spectrum uses 6430 triple quadrupole mass spectrometer of Agilent, and electron spray positive ion source react more
It monitors analytical model (MRM).
In (a) liquid phase chromatogram condition, chromatographic column is Agilent Poroshell 120SB-C18 chromatographic column (4.6mm
× 75mm, 2.7 μm), sample detection time: 6min；Flow velocity: 1.0ml/min；Sample volume: 5 μ l；Column temperature: 40 DEG C.
In (b) Mass Spectrometry Conditions, dry gas: N2；Dry gas stream speed: 10L/min, dry atmospheric pressure: 45psi is dry
Temperature degree: 350 DEG C, capillary voltage: 4000V.MRM monitoring method parameter is shown in Table 1.
1 arecaline of table and interior target mass spectrum monitoring parameters
The Arecoline hydrobromide reference substance stock solution: precision weighs Arecoline hydrobromide reference substance 15mg, sets 100ml amount
In bottle, add diluent to dissolve and be settled to scale, shake up, precision measures 1ml and sets in 10ml measuring bottle, adds diluent dissolution and constant volume
It to scale, shakes up, obtaining betel nut alkali content is about 10 μ g/ml reference substance stock solutions.Arecaline weight=Arecoline hydrobromide weight/
1.5214。
The internal standard stock solution: precision weighs diazepam 10mg, sets in 100ml measuring bottle, and diluent is added to dissolve and be settled to
Scale shakes up, and precision measures 1ml and sets in 10ml measuring bottle, adds diluent to dissolve and is settled to scale, shake up, obtains internal standard stock solution.
The diluent: 0.9% sodium chloride injection-methanol (50:50).
The 10mmol/l ammonium acetate solution: precision weighs ammonium acetate 0.7708g, sets in beaker, and precision measures water
1000ml, with formic acid tune pH to 5.2.
The present invention establishes measurement of the HPLC-MS/MS method for betel nut alkali content in children's indigestion tablet, and to its side of progress
Science of law verifying, the results showed that, the method established meets " the drug standard analysis method verification guide of Chinese Pharmacopoeia 2015 editions
Principle " requirement, test solution pre-treating method is easy to operate compared with HPLC method in method, and the operating time is short, and detection method is special
Attribute is strong, high sensitivity, stabilization, reliable, can be used for assay, the control of helping digestion of baby tablet quality of arecaline, to producing
Journey and drug safety provide beneficial reference.
Detailed description of the invention
The MRM mass spectrogram of Fig. 1 diluent.
The MRM mass spectrogram of Fig. 2 solution 5 (containing the internal standard).In figure: A- arecaline, B- internal standard.
The MRM mass spectrogram of Fig. 3 test solution.In figure: A- arecaline, B- internal standard.
Specific embodiment
Technical solution of the present invention is described in further detail with attached drawing combined with specific embodiments below.Following the description
It is merely to illustrate the present invention, but the present invention is not limited to this.
1 instrument and reagent
Agilent 1260-6430 liquid chromatography mass spectrometric combined system (LC-MS/MS), Anjelen Sci. & Tech. Inc, including
G1379B type degasser, G1312B type binary infusion pump, G1367E type autosampler, G1330B type temperature control module, G1316A
Type column oven, 6430MS/MS system and Mass hunter data acquisition software.FE20 plum Teller-support benefit pH meter, plum Teller-
Hold in the palm benefit instrument (Shanghai) Co., Ltd..AUW-120D type electronic analytical balance, Shimadzu Corporation.ME-204E type electronic analysis day
It is flat, Mettler-Toledo Instrument (Shanghai) Co., Ltd..Milli-Q ultrapure water machine, Merck Chemical Engineering Technology (Shanghai) limited public affairs
Department.KQ3200B type ultrasonic cleaner, Kunshan Ultrasonic Instruments Co., Ltd..LED heats magnetic stirring apparatus, BIOLOGIX.
Children's indigestion tablet (every slice weight 0.3g, provided by production unit).Arecoline hydrobromide (lot number: 111684-
200401, National Institute for Food and Drugs Control).Diazepam (IS) (lot number: 171225-201304, Chinese food drug assay
Research institute).Methanol (chromatographically pure, Merck).Ammonium acetate (LC/MS, Fisher scientific).Formic acid (LC/MS, Fisher
scientific).0.9% sodium chloride injection, water are the ultrapure water of Advantage A10 Milli-Q ultrapure water machine preparation.
The preparation of 2 solution
2.1 reference substance solutions are prepared
Diluent: 0.9% sodium chloride injection-methanol (50:50).
Solution 1 (reference substance stock solution): precision weighs Arecoline hydrobromide reference substance 15mg, sets in 100ml measuring bottle, adds dilute
It releases agent and dissolves and be settled to scale, shake up, precision measures 1ml and sets in 10ml measuring bottle, adds diluent to dissolve and is settled to scale, shakes
Even, obtaining betel nut alkali content is about 10 μ g/ml reference substance stock solutions.Arecaline weight=Arecoline hydrobromide weight/1.5214.
Solution 2 (internal standard stock solution): precision weighs diazepam 10mg, sets in 100ml measuring bottle, adds diluent dissolution and constant volume
It to scale, shakes up, precision measures 1ml and sets in 10ml measuring bottle, adds diluent to dissolve and is settled to scale, shake up, obtains in 10 μ g/ml
Mark stock solution.
Calibration curve solution: precision measures solution 1, solution 2 in right amount, until adding diluent quantitatively to dilute in EP pipe and being made one
Series standard curve solution (table 2).
2 calibration curve solution of table
2.2 test solutions are prepared
If taking this product dry plate, about 0.6g is taken after finely ground, it is accurately weighed, it sets in 25ml volumetric flask, adds 0.9% chloride injection
Liquid is settled to scale, sets on magnetic stirring apparatus with 850r/min revolving speed, stirs 5min.It is mixed for 24mg/ml test sample up to concentration
Suspension.
Precision pipettes test sample suspension 3ml, sets in EP pipe, after ultrasonic 30min, 0.22 μm of MICRO PES polyether sulfone water
Mesentery filtering, it is accurate respectively to measure 500 μ l of subsequent filtrate, 10 μ l of 490 μ l of methanol and solution 2 (internal standard stock solution), it sets in EP pipe, mixes
It is even, as test solution.
3 methodology validations
3.1 liquid phase chromatogram condition liquid phases use 1260 efficient liquid phase of Agilent, chromatographic column: Agilent Poroshell
120SB-C18 chromatographic column (4.6mm × 75mm, 2.7 μm)；Mobile phase: A:10mmol/l ammonium acetate solution is (extremely with formic acid tune pH
5.2)；B: methanol.Type of elution: gradient elution；Gradient program is as follows: 0~0.5min, 15% (v/v) B；2.1~
3.0min, 90% (v/v) B；3.1~6min, 15% (v/v) B.Sample detection time: 6min；Flow velocity: 1.0ml/min；Sample introduction
Amount: 5 μ l；Column temperature: 40 DEG C.
Mass Spectrometry Conditions mass spectrum uses 6430 triple quadrupole mass spectrometer of Agilent, electron spray positive ion source, more reaction prisons
It surveys analytical model (MRM).Dry gas: N2；Dry gas stream speed: 10L/min, dry atmospheric pressure: 45psi, dry temperature degree: 350
DEG C, capillary voltage: 4000V.Quota ion pair arecaline: [M+H]+M/z 156.1/44.2, fragment voltage: 100V, collision
Energy: 13eV；Internal standard diazepam: [M+H]+M/z 285.1/193.1, fragment voltage: 150V, collision energy: 30eV.
3.2 specificity
Take solution 5 (containing the internal standard), solution 5 (not containing the internal standard), the diluent, inner mark solution (internal standard in calibration curve solution
Stock solution dilute 100 times be made), test solution by 3.1 methods detection, obtain mass spectrogram (see Fig. 1).The result shows that test sample
With reference substance appearance position consistency, it is noiseless that internal standard and reference substance go out peak position, and in peak position out, blank solvent not appearance.
3.3 linear and ranges
The reference substance serial solution prepared under 2.1 is taken, is detected by 3.1 methods.Using the concentration of arecaline as abscissa X,
The peak area ratio of arecaline and internal standard compound is ordinate Y, with weighted least-squares method (weight 1/X2) regressing calculation is carried out,
The linear equation acquired is standard curve.Regression equation is Y=0.173930X+0.001489；R=0.9979.Arecaline exists
Linear relationship is good within the scope of 50~2000ng/ml.
Reference substance solution is taken to dilute step by step, it is true by signal-to-noise ratio (S/N) 3:1 by measurement peak height (S) and baseline noise (N)
Regular inspection rising limit is 1.5ng/ml, determines by signal-to-noise ratio (S/N) 10:1 and minimum is quantitatively limited to 5ng/ml.
3.4 precision
Repeatability: taking with a test solution, according to 3.1 methods, continuous sample introduction 6 times, and arecaline in computer chromatography figure
RSD with internal standard peak area ratio is 1.6%, < 5%.
Intermediate precision: according to 2.2 operations, another test solution was prepared in the 2nd day, by 3.1 methods, continuous sample introduction
6 times, the RSD of arecaline and internal standard peak area ratio is 1.1%, < 5% in computer chromatography figure.
Show that method precision meets the requirements.
3.5 the rate of recovery
The same a collection of test sample of known content is taken, finely ground rear accurately weighed, every part of about 0.6g, 3 parts are one group, are separately added into
A certain amount of reference substance stock solution makes with 3 groups of content ratio of arecaline in test sample to be respectively 1:1.5,1:1,1:0.5, press
According to test solution is prepared under 2.2, detected by 3.1 methods.It the results are shown in Table 3, show that the sample treatment rate of recovery is stablized.
3 rate of recovery experimental result of table
3.6 study on the stability
The test sample suspension for being used for repeated experiment under precision item is taken, at room temperature, 4h is placed, respectively 0,2,4h
The parallel sampling in the middle part of solution is corresponding test solution by 2.2 lower method processing, detects by 3.1 methods, record peak face
Long-pending, the RSD of arecaline and internal standard peak area ratio is 4.9% in computer chromatography figure, shows test solution in 4h internal stability
Well.
Claims (5)
1. a kind of method of betel nut alkali content in LC-MS quantitative detection children's indigestion tablet, which is characterized in that including step (1)
Sample preparation, the preparation of (2) standard curve, (3) detect betel nut alkali content using liquid chromatograph mass spectrography；
(1) takes about 0.6g if the step of sample preparation includes: to take this product dry plate after finely ground, accurately weighed, sets 25ml measuring bottle
In, add 0.9% sodium chloride injection to be settled to scale, sets on magnetic stirring apparatus with 850r/min revolving speed, stir 5min；Up to dense
Degree is 24mg/ml test sample suspension；
Precision pipettes test sample suspension 3ml, sets in EP pipe, after ultrasonic 30min, 0.22 μm of MICRO PES polyether sulfone water system film
Filtering, precision measure 500 μ l of subsequent filtrate, 10 μ l of 490 μ l of methanol and internal standard stock solution, set in EP pipe, mix, as test sample into
Sample solution；
Diazepam is designated as in the internal standard stock solution；
The step of prepared by (2) standard curve, which includes: that difference is accurate, measures Arecoline hydrobromide reference substance stock solution 5,20,
50,100,200 μ l, and it is separately added into 10 μ l of internal standard stock solution, supplying diluent is in right amount 1000 μ l to final volume, and a system is made
Column calibration curve solution is detected using the method for (3) liquid chromatograph mass spectrography detection, records the hydrobromic acid Bin of each concentration
The corresponding peak area of bulky alkali；Using Arecoline hydrobromide and interior target peak area ratio as ordinate, with the dense of Arecoline hydrobromide
Degree is abscissa X, prepares the equation of linear regression of Arecoline hydrobromide；
Described (3) include: using the step of liquid chromatograph mass spectrography detection
(a) liquid phase chromatogram condition chromatographic column: C18 column；Mobile phase: A:10mmol/l ammonium acetate solution, with formic acid tune pH to 5.2；
B: methanol；Type of elution: gradient elution；Gradient program is as follows: 0~0.5min, with volume ratio 15%B；2.1~
3.0min, with volume ratio 90%B；3.1~6min, with volume ratio 15%B；
(b) Mass Spectrometry Conditions mass spectrum uses 6430 triple quadrupole mass spectrometer of Agilent, electron spray positive ion source, multiple-reaction monitoring
Analytical model (MRM)；
In (a) liquid phase chromatogram condition, chromatographic column be Agilent Poroshell 120SB-C18 chromatographic column, 4.6mm ×
75mm, 2.7 μm, sample detection time: 6min；Flow velocity: 1.0ml/min；Sample volume: 5 μ l；Column temperature: 40 DEG C；
In (b) Mass Spectrometry Conditions, dry gas: N2；Dry gas stream speed: 10L/min, dry atmospheric pressure: 45psi, dry temperature
Degree: 350 DEG C, capillary voltage: 4000V；Quota ion pair arecaline: [M+H]+M/z 156.1/44.2, fragment voltage:
100V, collision energy: 13eV；Internal standard diazepam: [M+H]+M/z 285.1/193.1, fragment voltage: 150V, collision energy:
30eV。
2. the method for betel nut alkali content, special in a kind of LC-MS quantitative detection children's indigestion tablet as described in claim 1
Sign is that the Arecoline hydrobromide reference substance stock solution: precision weighs Arecoline hydrobromide reference substance 15mg, sets 100ml amount
In bottle, add diluent to dissolve and be settled to scale, shake up, precision measures 1ml and sets in 10ml measuring bottle, adds diluent dissolution and constant volume
It to scale, shakes up, obtaining betel nut alkali content is about 10 μ g/ml reference substance stock solutions；Arecaline weight=Arecoline hydrobromide weight/
1.5214。
3. the method for betel nut alkali content, special in a kind of LC-MS quantitative detection children's indigestion tablet as described in claim 1
Sign is that the internal standard stock solution: precision weighs diazepam 10mg, sets in 100ml measuring bottle, adds diluent to dissolve and is settled to quarter
Degree, shakes up, and precision measures 1ml and sets in 10ml measuring bottle, adds diluent to dissolve and is settled to scale, shake up, obtains internal standard stock solution.
4. the method for betel nut alkali content, special in a kind of LC-MS quantitative detection children's indigestion tablet as described in claim 1
Sign is, the diluent: 0.9% sodium chloride injection-methanol, with volume ratio 50:50.
5. the method for betel nut alkali content, special in a kind of LC-MS quantitative detection children's indigestion tablet as described in claim 1
Sign is that the 10mmol/l ammonium acetate solution: precision weighs ammonium acetate 0.7708g, sets in beaker, and precision measures water
1000ml, with formic acid tune pH to 5.2.
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| CN102346177B (en) * | 2011-05-13 | 2013-11-27 | 湖南汉森制药股份有限公司 | Method for detecting Simotang preparation |
| CN103940935A (en) * | 2013-01-23 | 2014-07-23 | 中国农业科学院兰州畜牧与兽药研究所 | Concentration determining method of arecoline hydrobromide in animal blood plasma |
| CN104749281B (en) * | 2015-04-03 | 2016-08-24 | 山东宏济堂制药集团股份有限公司 | A kind of detection method of helping digestion of baby medicine |
| CN105738551B (en) * | 2016-04-22 | 2017-09-22 | 云南中烟工业有限责任公司 | A kind of detection method of arecaline |
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