CN111077246A - Method for detecting 4-methoxy o-phenylenediamine by using ultra-high performance liquid chromatography-tandem mass spectrometry - Google Patents
Method for detecting 4-methoxy o-phenylenediamine by using ultra-high performance liquid chromatography-tandem mass spectrometry Download PDFInfo
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Abstract
The invention relates to a method for detecting 4-methoxy o-phenylenediamine by using ultra-high performance liquid chromatography-tandem mass spectrometry, which comprises the following steps: taking 0.01-0.05 g of a to-be-detected product, accurately measuring the to-be-detected product to 0.01mg, placing the to-be-detected product in a volumetric flask, adding acetonitrile-water (3-8): 6 to 20-50ml of constant volume, carrying out vortex mixing for 2-10 min, carrying out ultrasonic extraction for 2-10 min, filtering the mixture through a 0.22 mu m filter membrane, and carrying out sample introduction to detect 4-methoxy o-phenylenediamine in the sample; step (2), detection conditions: the method adopts an ultra performance liquid chromatography-tandem mass spectrometry UPLC-MS/MS as a detection instrument to detect the 4-methoxy o-phenylenediamine. The invention can simply, quickly and efficiently carry out qualitative and quantitative detection on the 4-methoxy o-phenylenediamine in the pharmaceutical raw material medicines, the agricultural chemicals and the foods by using the UPLC-MS/MS.
Description
Technical Field
The invention relates to a detection method of 4-methoxy o-phenylenediamine, in particular to a method for detecting 4-methoxy o-phenylenediamine by using ultra-high performance liquid chromatography-tandem mass spectrometry.
Background
With the development of society and the advancement of science and technology. Human beings pay more and more attention to health, and medicines play a vital role in ensuring human health. Therefore, the pharmaceutical industry has become one of the most important areas of society. How to accurately and rapidly detect potentially low-limiting amounts of hazardous substances in pharmaceutical agents is a challenge facing the pharmaceutical industry today. The application of advanced modern instrumental analysis technology to meet the challenge is of great significance to the promotion of the safety evaluation of the medicine and the improvement of the commercial value of the medicine.
The instrument analysis is taken as a modern detection main means and is widely applied to the detection in the fields of chemistry, medicines, foods, cosmetics, agricultural chemicals and the like. Instrumental analysis enables the determination of the composition, content of the components and chemical structure of a substance by measuring several physicochemical properties, parameters and changes thereof. With the progress of the scientific technology of instrumental analysis, more and more advanced instrumental analysis techniques are widely applied to various detection fields, wherein the mass spectrometry detection technique is one of the techniques. The mass spectrometry detection is to ionize each component in a sample in an ion source to generate charged ions with different mass-to-charge ratios, after the ions are formed under the action of an accelerating electric field, the ions enter a mass analyzer, and after mass spectrometry signals are detected by the mass analyzer, visible spectrograms are formed on computer software through electronic conversion to be analyzed and researched by scientific research technicians. In order to combine the advantages of chromatographic separation, mass spectrometry is generally used in conjunction with chromatography, resulting in a chromatography-mass spectrometry technique. The chromatography-mass spectrometry combined technology has the advantages of both chromatography and mass spectrometry, namely good selectivity, high sensitivity, less test dosage, easy operation, high analysis speed, good reproducibility, small error, accuracy, reliability and the like. According to different chromatographic techniques, the chromatographic-mass spectrometry technology can be divided into LC-MS and GC-MS. The UPLC-MS/MS is one of the LC-MS used in the invention, the method adopts the tandem mass spectrum as a mass spectrum detector, and is formed by connecting three stages of mass spectrums in series, so that the selectivity of target ions can be effectively improved, the noise interference can be reduced, the signal-to-noise ratio can be further improved, and the detection limit can be further reduced, and the UPLC has the advantages of high separation efficiency, high separation speed, less used reagent and the like. In view of the great advantages of the UPLC-MS/MS technology, the technology is widely applied to the fields of medicines, chemistry, food science, cosmetics and the like.
The 4-methoxy o-phenylenediamine is one of raw materials for preparing the medicine esomeprazole and is a potential genotoxic substance. After being inhaled by human body, the medicine has the risk of causing gene mutation and further causing canceration, and finally seriously endangers human health. Therefore, in order to ensure the safety of the medicine esomeprazole, the residual quantity of 4-methoxy o-phenylenediamine in the medicine esomeprazole reagent must be strictly controlled.
Because 4-methoxy o-phenylenediamine has low boiling point, small molecular weight, weak ultraviolet absorption and more heteroatoms, the detection of the low concentration limit of 4-methoxy o-phenylenediamine in a sample by using common detection methods such as GC-FID, HPLC-UV and GC-MS is difficult.
At present, an ultra-high performance liquid chromatography-tandem mass spectrometry combined method which has high density, is simple, rapid and easy to operate and is used for effectively detecting the residual 4-methoxy o-phenylenediamine in the medicine is lacked.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for detecting 4-methoxy o-phenylenediamine by using ultra-high performance liquid chromatography-tandem mass spectrometry, which has good selectivity and high detection sensitivity.
The technical scheme for realizing the purpose of the invention is as follows: a method for detecting 4-methoxy o-phenylenediamine by using ultra-high performance liquid chromatography-tandem mass spectrometry comprises the following steps:
putting a sample to be detected into a volumetric flask, adding acetonitrile-water (3-8): 6 to a constant volume of 20-50ml, carrying out vortex mixing for 2-10 min, carrying out ultrasonic extraction for 2-10 min, filtering through a 0.22 mu m filter membrane, and carrying out sample injection to detect 4-methoxy o-phenylenediamine in the sample;
step (2), detection conditions: the method adopts an ultra performance liquid chromatography-tandem mass spectrometry UPLC-MS/MS as a detection instrument to detect the 4-methoxy o-phenylenediamine.
According to the technical scheme, in the step (1), 0.01-0.05 g of a sample to be detected is taken, the sample is accurately measured to be 0.01mg, the sample is placed in an empty volumetric flask, acetonitrile-water (3-8): 6 is added, the volume is constant to be 20-50ml, vortex mixing is carried out for 2-10 min, ultrasonic extraction is carried out for 2-10 min, and the sample is filtered through a 0.22 mu m filter membrane.
In the step (2), the data acquisition mode of the ultra-high performance liquid chromatography-tandem mass spectrometer is to select reaction detection (SRM) and select mass-to-charge ratio
m/z 139.15 → 122.1 as a qualitative and quantitative ion pair;
in the step (2), the chromatographic column of the ultra-high performance liquid chromatography-tandem mass spectrometer is a high performance liquid chromatographic column taking C18 bonded silica gel as a stationary phase: the length of the amino column is 100-150 mm, the column diameter is 4.6mm, and the particle size of the filler is 2.6 mu m;
in the technical scheme, in the step (2), the flow rate of the ultra-high performance liquid chromatography-tandem mass spectrometer is 0.2-1.0 ml/min;
in the technical scheme, in the step (2), the column temperature of the ultra-high performance liquid chromatography-tandem mass spectrometry combination instrument is 25-45 ℃;
in the technical scheme, in the step (2), the sample injection volume of the ultra-high performance liquid chromatography-tandem mass spectrometry instrument is 1-10 mu L;
in the step (2), the mass spectrum condition of the ultra-high performance liquid chromatography-tandem mass spectrometer is HESI+The ion source comprises an ion source, wherein the capillary tube voltage is 2800-3800 v, the capillary tube temperature is 250-380 ℃, the ion source temperature is 150-350 ℃, the atomizing gas is nitrogen, the sheath gas pressure is 30-100 psi, the auxiliary gas pressure is 0-10 psi, the ion transmission voltage is 40-100 v, the collision gas is argon, the collision gas pressure is 1.0-2.0 mtorr, the collision energy is 5 v-30 v respectively, and the scanning time is 0.1-1.0 s.
After the technical scheme is adopted, the invention has the following positive effects:
the detection method has the advantages of good selectivity, high sensitivity, simplicity, rapidness and the like. According to the invention, the UPLC-MS/MS is used for quickly and efficiently carrying out limited test on 4-methoxy o-phenylenediamine in bulk drugs, pharmaceutical preparations and other samples; the detection sensitivity of the 4-methoxy o-phenylenediamine can be effectively improved, the matrix interference is effectively avoided, the detection limit of the 4-methoxy o-phenylenediamine is reduced, and the lowest detection limit is 2.5 ng/mL; the limit of quantitation is 5.1 ng/mL; the linear correlation coefficient is 0.999 within the concentration range of 5.1 ng/mL-84.6 ng/mL.
Drawings
In order that the present disclosure may be more readily and clearly understood, reference is now made to the following detailed description of the present disclosure taken in conjunction with the accompanying drawings, in which
FIG. 1 is a qualitative and quantitative ion chromatogram of a 4-methoxy-o-phenylenediamine standard of the present invention;
FIG. 2 is a mass spectrum of a 4-methoxy o-phenylenediamine standard of the present invention;
FIG. 3 is a qualitative and quantitative ion chromatogram of a blank solvent of the present invention;
FIG. 4 is a mass spectrum of a blank solvent of the present invention;
FIG. 5 is a qualitative and quantitative ion chromatogram of a blank sample extract according to the present invention;
FIG. 6 is a mass spectrum of a blank sample extract of the present invention;
FIG. 7 is a qualitative and quantitative ion chromatogram of a sample spiked in accordance with the present invention;
FIG. 8 is a mass spectrum of a sample of the present invention with a label;
FIG. 9 is a qualitative and quantitative ion chromatogram of a 2.5ng/mL 4-methoxyphenylenediamine standard of the present invention;
FIG. 10 is a mass spectrum of a 2.5ng/mL 4-methoxy-o-phenylenediamine standard of the present invention;
FIG. 11 is a qualitative and quantitative ion chromatogram of a 5.1ng/mL 4-methoxyphenylenediamine standard of the present invention;
FIG. 12 is a mass spectrum of a 5.1ng/mL 4-methoxy-o-phenylenediamine standard of the present invention;
FIG. 13 is a qualitative and quantitative ion chromatogram of a 6.3ng/mL 4-methoxyphenylenediamine standard of the present invention;
FIG. 14 is a mass spectrum of a 6.3ng/mL 4-methoxy-o-phenylenediamine standard of the present invention;
FIG. 15 is a qualitative and quantitative ion chromatogram of a 12.7ng/mL 4-methoxyphenylenediamine standard of the present invention;
FIG. 16 is a mass spectrum of a 12.7ng/mL 4-methoxy-o-phenylenediamine standard of the present invention;
FIG. 17 is a qualitative and quantitative ion chromatogram of a 19.0ng/mL 4-methoxyphenylenediamine standard of the present invention;
FIG. 18 is a mass spectrum of a 19.0ng/mL 4-methoxy-o-phenylenediamine standard of the present invention;
FIG. 19 is a qualitative and quantitative ion chromatogram of a 38.1ng/mL 4-methoxyphenylenediamine standard of the present invention;
FIG. 20 is a mass spectrum of a 38.1ng/mL 4-methoxy-o-phenylenediamine standard of the present invention;
FIG. 21 is a qualitative and quantitative ion chromatogram of an 84.6ng/mL 4-methoxyphenylenediamine standard of the present invention.
FIG. 22 is a mass spectrum of 84.6ng/mL 4-methoxy-o-phenylenediamine standards of the present invention;
FIG. 23 is a standard graph of a linearity experiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Example 1
The invention provides a method for detecting 4-methoxy o-phenylenediamine by using ultra-high performance liquid chromatography-tandem mass spectrometry, which comprises the following steps:
putting a sample to be detected into a volumetric flask, adding acetonitrile-water (3-8): 6 to a constant volume of 20-50ml, carrying out vortex mixing for 2-10 min, carrying out ultrasonic extraction for 2-10 min, filtering through a 0.22 mu m filter membrane, and carrying out sample injection to detect 4-methoxy o-phenylenediamine in the sample;
step (2), detection conditions: the method adopts an ultra performance liquid chromatography-tandem mass spectrometry UPLC-MS/MS as a detection instrument to detect the 4-methoxy o-phenylenediamine.
In the step (1), 0.02g of sample to be detected is taken, the sample is accurate to 0.01mg, the sample is placed in an empty volumetric flask, acetonitrile-water 4:6 is added, the volume is fixed to 20ml, vortex mixing is carried out for 10min, ultrasonic extraction is carried out for 5min, and the sample passes through a 0.22 mu m filter membrane.
In the step (2), the data acquisition mode of the ultra performance liquid chromatography-tandem mass spectrometer is to select a reaction detection SRM, and select a mass-to-charge ratio m/z of 139.15 → 121.1 as a qualitative and quantitative ion pair; the chromatographic column of the ultra-high performance liquid chromatography-tandem mass spectrometry instrument is a high performance liquid chromatographic column taking C18 bonded silica gel as a stationary phase: c18 column length 100mm, column diameter 4.6mm, filler particle size 2.6 μm; the flow rate of the ultra-high performance liquid chromatography-tandem mass spectrometry instrument is 0.4 ml/min; the column temperature of the ultra-high performance liquid chromatography-tandem mass spectrometry instrument is 30 ℃; the sample injection volume of the ultra-high performance liquid chromatography-tandem mass spectrometry instrument is 5 mu L; the mass spectrum condition of the ultra-high performance liquid chromatography-tandem mass spectrometer is HESI+The ion source comprises an ion source, wherein the capillary tube voltage is 2800-3800 v, the capillary tube temperature is 250-380 ℃, the ion source temperature is 150-350 ℃, the atomizing gas is nitrogen, the sheath gas pressure is 40psi, the auxiliary gas pressure is 5psi, the ion transmission voltage is 40-100 v, the collision gas is argon, the collision gas pressure is 1.0-2.0 mtorr, the collision energy is 5-30 v, and the scanning time is 0.5 second.
The following test samples were provided by coffepin pharmaceuticals, inc.
Blank test and specificity test:
as shown in FIGS. 1 to 2, about 22mg of 4-methoxy-o-phenylenediamine standard was weighed into a 100ml volumetric flask, dissolved with acetonitrile-water 4:6 and fixed to the scale. Diluting the 4-methoxy o-phenylenediamine standard solution to 5.1ng/mL by using acetonitrile-water 4:6, and then sampling 1.5mL in a sampling vial for analysis to obtain a chromatogram of the 4-methoxy o-phenylenediamine standard. As shown in fig. 3 to 4, are chromatograms of acetonitrile-water 4:6 solvent. 1ml acetonitrile-water 4:6 solvent is taken for sample injection analysis. And the non-interference peak is arranged at the position of the checked target peak.
As shown in fig. 5 to fig. 6, about 19mg esomeprazole solid powder is respectively weighed into a 20ml volumetric flask, an appropriate amount of acetonitrile-water 4:6 is added, vortex mixing is carried out for 10min, ultrasonic extraction is carried out for 5min, acetonitrile-water 4:6 is used for constant volume till the volume is scaled, and the mixture is uniformly mixed. 2ml of the solution was applied to a 0.22 μm filter and analyzed by injection. And the non-interference peak is arranged at the position of the checked target peak.
Comparing the blank solvent chromatogram and the blank sample chromatogram with the 4-methoxy o-phenylenediamine standard chromatogram to see that the blank solvent of acetonitrile-water 4:6 and the blank matrix of the sample have no interference peak at the target peak position for 1.5-2.5 min; thus, it is believed that the solvent and sample matrix do not interfere with the 4-methoxy-o-phenylenediamine detection.
Linear experiments:
as shown in fig. 11, 13, 15, 17, 19 and 21, about 22mg of the 4-methoxy-o-phenylenediamine standard was weighed into a 100ml volumetric flask, dissolved in acetonitrile-water 4:6 and fixed to a scale. Diluting the 4-methoxy o-phenylenediamine standard solution with acetonitrile-water 4:6 to prepare a series of standard solutions, and carrying out sample injection analysis. The peak area was plotted against concentration to obtain a linear result. The experimental data obtained are shown in table 1 below, and table 1 is the standard sequence experimental determination data:
TABLE 1
As shown in fig. 21, a standard graph of a linear experiment. The response value of the 4-methoxy o-phenylenediamine instrument shows a good linear relation in 5.1 ng/mL-84.6 ng/mL, and the linear correlation coefficient is as follows: 0.999, the requirement of detection is met.
The detection limit and the quantification limit are shown in figure 9 and figure 11, and the chromatogram and the mass spectrum of the standard product of 2.5ng/mL 4-methoxy o-phenylenediamine are shown; the signal-to-noise ratio of the detection signal reaches the detection limit requirement of S/N >3 at 1.5-2.5 min, wherein the signal-to-noise ratio is 29. 5.1ng/mL 4-methoxy o-phenylenediamine standard chromatogram and mass spectrum; the signal-to-noise ratio of the method reaches the quantitative limit requirement of S/N >10 at 1.5-2.5 min, wherein the signal-to-noise ratio is 100.
Precision:
and selecting a 4-methoxy o-phenylenediamine concentration point to perform 6 repeated experiments, wherein 455ng/mL is selected as the concentration of the 4-methoxy o-phenylenediamine standard solution for the precision experiment. The specific data are shown in the following table 2, and the table 2 is the precision experimental data of 4-methoxy o-phenylenediamine:
TABLE 2
As can be seen from the data shown in Table 2, the precision of the experiment can meet the detection requirements.
Standard addition recovery experiment:
three standard adding concentrations are selected in the experiment to carry out three parallel tests respectively, and the standard adding concentrations are as follows: 6.6mg/kg, 13.4mg/kg, 20.0mg/kg i.e. 6.3ng/mL, 12.7ng/mL, 19.0 ng/mL. The experimental data are shown in the following table 3, and the table 3 is the experimental data of the standard addition recovery of the 4-methoxy o-phenylenediamine.
TABLE 3
As shown in Table 3, the recovery rate is 60-130% by adding the standard of 4-methoxy o-phenylenediamine, which meets the test requirements.
Example 2
Example 2 differs from example 1 in that: adding acetonitrile-water 7:6 to 25ml, carrying out vortex oscillation for 10min, carrying out ultrasonic extraction for 6min, filtering through a 0.22 mu m filter membrane, and carrying out sample injection to detect 4-methoxy o-phenylenediamine in a sample; taking a sample to be detected as 0.025g, accurately measuring to 0.01mg, placing in an empty volumetric flask, adding acetonitrile-water 7:6 to a constant volume of 25ml, mixing for 10min by vortex, and extracting for 6min by ultrasonic.
Example 3
Example 3 differs from example 1 in that: adding acetonitrile-water 7:6 to 50ml, carrying out vortex oscillation for 10min, carrying out ultrasonic extraction for 8min, filtering through a 0.22 mu m filter membrane, and carrying out sample injection to detect 4-methoxy o-phenylenediamine in a sample; taking a sample to be detected as 0.049g, accurately measuring to 0.01mg, placing in an empty volumetric flask, adding acetonitrile-water 7:6 to a constant volume of 50ml, carrying out vortex mixing for 10min, and carrying out ultrasonic extraction for 8 min.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method for detecting 4-methoxy o-phenylenediamine by using ultra-high performance liquid chromatography-tandem mass spectrometry is characterized by comprising the following steps:
putting a sample to be detected into a volumetric flask, adding acetonitrile-water (3-8): 6 to a constant volume of 20-50ml, carrying out vortex mixing for 2-10 min, carrying out ultrasonic extraction for 2-10 min, filtering through a 0.22 mu m filter membrane, and carrying out sample injection to detect 4-methoxy o-phenylenediamine in the sample;
step (2), detection conditions: the method adopts an ultra performance liquid chromatography-tandem mass spectrometry UPLC-MS/MS as a detection instrument to detect the 4-methoxy o-phenylenediamine.
2. The method for detecting 4-methoxy o-phenylenediamine by using ultra-high performance liquid chromatography-tandem mass spectrometry as claimed in claim 1, wherein: in the step (1), 0.01-0.05 g of a sample to be detected is taken, and the accuracy is 0.01 mg.
3. The method for detecting 4-methoxy o-phenylenediamine by using ultra-high performance liquid chromatography-tandem mass spectrometry as claimed in claim 1, wherein: in the step (2), the data acquisition mode of the ultra-high performance liquid chromatography-tandem mass spectrometer is to select a reaction detection SRM and select a mass-to-charge ratio
m/z 139.15 → 122.1 as a qualitative and quantitative ion pair.
4. The method for detecting 4-methoxy o-phenylenediamine by using ultra-high performance liquid chromatography-tandem mass spectrometry as claimed in claim 1, wherein: in the step (2), the chromatographic column of the ultra-high performance liquid chromatography-tandem mass spectrometer is a high performance liquid chromatographic column taking C18 bonded silica gel as a stationary phase: the length of the amino column is 100-150 mm, the column diameter is 4.6mm, and the particle size of the filler is 2.6 mu m.
5. The method for detecting 4-methoxy o-phenylenediamine by using ultra-high performance liquid chromatography-tandem mass spectrometry as claimed in claim 1, wherein: in the step (2), the flow rate of the ultra-high performance liquid chromatography-tandem mass spectrometry instrument is 0.2-1.0 ml/min.
6. The method for detecting 4-methoxy o-phenylenediamine by using ultra-high performance liquid chromatography-tandem mass spectrometry as claimed in claim 1, wherein: in the step (2), the column temperature of the ultra-high performance liquid chromatography-tandem mass spectrometry instrument is 25-45 ℃.
7. The method for detecting 4-methoxy o-phenylenediamine by using ultra-high performance liquid chromatography-tandem mass spectrometry as claimed in claim 1, wherein: in the step (2), the sample injection volume of the ultra-high performance liquid chromatography-tandem mass spectrometry instrument is 1-10 mu L.
8. The method for detecting 4-methoxy o-phenylenediamine by using ultra-high performance liquid chromatography-tandem mass spectrometry as claimed in claim 1, wherein: in the step (2), the mass spectrum condition of the ultra-high performance liquid chromatography-tandem mass spectrometer is HESI+The ion source comprises an ion source, wherein the capillary tube voltage is 2800-3800 v, the capillary tube temperature is 250-380 ℃, the ion source temperature is 150-350 ℃, the atomizing gas is nitrogen, the sheath gas pressure is 30-100 psi, the auxiliary gas pressure is 0-10 psi, the ion transmission voltage is 40-100 v, the collision gas is argon, the collision gas pressure is 1.0-2.0 mtorr, the collision energy is 5 v-30 v respectively, and the scanning time is 0.1-1.0 s.
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