CN110988151A - Method for detecting chloroacetic acid by using ultra-high performance liquid chromatography-tandem mass spectrometry - Google Patents
Method for detecting chloroacetic acid 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 chloroacetic acid by using ultra-high performance liquid chromatography-tandem mass spectrometry, which comprises the following steps: a method for detecting chloroacetic acid 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 in a ratio of 1: 1-9: 1 to a constant volume of 10-50 ml, carrying out vortex mixing for 5-15 min, carrying out ultrasonic extraction for 5-15 min, filtering through a 0.22 mu m filter membrane, and carrying out sample injection to detect chloroacetic acid in the sample; and (2) detecting chloroacetic acid by using an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) as a detection instrument. In the step (1), 0.1-0.5 g of the product to be detected is taken, the precision is 0.01mg, the product is placed in an empty volumetric flask, acetonitrile-water is added, the volume is fixed to 10-50 ml in a ratio of 1: 1-9: 1, vortex mixing is carried out for 5-15 min, ultrasonic extraction is carried out for 5-15 min, and the product is filtered through a 0.22 mu m filter membrane. The UPLC-MS/MS is used for simply, quickly and efficiently carrying out qualitative and quantitative detection on chloroacetic acid in pharmaceutical raw material medicines, agricultural chemicals and food.
Description
Technical Field
The invention relates to a method for detecting chloroacetic acid, in particular to a method for detecting chloroacetic acid 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.
Chloroacetic acid is a toxic substance. After being inhaled by human body, the medicine can cause bronchitis, pulmonary edema and skin damage, and in severe cases, the medicine can cause excessive saliva, deep breath, cough, nausea and vomiting, and finally endanger life safety. Therefore, the residual amount of chloroacetic acid in the pharmaceutical agent must be strictly controlled in order to ensure the safety of the drug.
Due to the low boiling point, small molecular weight, weak ultraviolet absorption and small proportion of carbon and hydrogen contained in the chloroacetic acid, the detection of the low concentration limit of the chloroacetic acid in the sample by using the commonly used 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 chloroacetic acid 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 chloroacetic acid by using ultra-high performance liquid chromatography-tandem mass spectrometry, which has the advantages of good selectivity, high detection sensitivity and high speed.
The technical scheme for realizing the purpose of the invention is as follows: a method for detecting chloroacetic acid 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 in a ratio of 1: 1-9: 1 to a constant volume of 10-50 ml, carrying out vortex mixing for 5-15 min, carrying out ultrasonic extraction for 5-15 min, filtering through a 0.22 mu m filter membrane, and carrying out sample injection to detect chloroacetic acid in the sample;
and (2) detecting chloroacetic acid by using an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) as a detection instrument.
In step (2), the data acquisition mode of the hplc-tandem mass spectrometer is to select a reaction detection SRM, and select a mass-to-charge ratio m/z 93 → 93, and m/z 93 → 77 as a qualitative and quantitative ion pair.
Further, in the step (2), the chromatographic column of the ultra performance liquid chromatography-tandem mass spectrometer is-NH2High performance liquid chromatography column with bonded silica gel as 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 3.5 mu m.
Further, in the step (2), the flow rate of the ultra-high performance liquid chromatography-tandem mass spectrometry instrument is 0.2-1.0 ml/ml.
Further, in the step (2), the column temperature of the ultra-high performance liquid chromatography-tandem mass spectrometry instrument is 25-45 ℃.
Further, in the step (2), the sample injection volume of the ultra-high performance liquid chromatography-tandem mass spectrometry instrument is 2-20 μ L.
Further, in the step (2), the mass spectrum conditions of the ultra-high performance liquid chromatography-tandem mass spectrometer are that an HESI ion source is adopted, the capillary tube voltage is 2800-3800 v, the capillary tube temperature is 250-380 ℃, the ion source temperature is 130-250 ℃, 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-40-90 v, the collision gas is argon, the collision gas pressure is 1.0-2.0 mtorr, the collision energy is respectively-5 v-30 v, and the scanning time is 0.1-1.0 seconds.
Further, in the step (1), the sample to be detected is 0.1-0.5 g, and the accuracy is 0.01 mg.
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. The UPLC-MS/MS can be used for quickly and efficiently carrying out limited test on chloroacetic acid in bulk drugs, pharmaceutical preparations and other samples; the detection sensitivity of the chloroacetic acid can be effectively improved, the matrix interference is effectively avoided, the detection limit of the chloroacetic acid is reduced, and the lowest detection limit is 91 ng/mL; the limit of quantitation is 227 ng/mL; the linear correlation coefficient is 0.999 within the concentration range of 227 ng/mL-911 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 chloroacetic acid standard of the present invention;
FIG. 2 is a mass spectrum of chloroacetic acid 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 91ng/mL chloroacetic acid standard of the present invention;
FIG. 10 is a mass spectrum of a 91ng/mL chloroacetic acid standard of the present invention;
FIG. 11 is a qualitative and quantitative ion chromatogram of 227ng/mL chloroacetic acid standard of the present invention;
FIG. 12 is a mass spectrum of 227ng/mL chloroacetic acid standard of the present invention;
FIG. 13 is a qualitative and quantitative ion chromatogram of a 328ng/mL chloroacetic acid standard of the present invention;
FIG. 14 is a mass spectrum of a 328ng/mL chloroacetic acid standard of the present invention;
FIG. 15 is a qualitative and quantitative ion chromatogram of 455ng/mL chloroacetic acid standard of the present invention;
FIG. 16 is a mass spectrum of 455ng/mL chloroacetic acid standard of the present invention;
FIG. 17 is a qualitative and quantitative ion chromatogram of a 683ng/mL chloroacetic acid standard of the present invention;
FIG. 18 is a mass spectrum of 683ng/mL chloroacetic acid standard according to the present invention;
FIG. 19 is a qualitative and quantitative ion chromatogram of a 911ng/mL chloroacetic acid standard of the present invention;
FIG. 20 is a mass spectrum of a 911ng/mL chloroacetic acid standard of the present invention;
FIG. 21 is a standard graph of a linear 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 chloroacetic acid 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 in a ratio of 1: 1-9: 1 to a constant volume of 10-50 ml, carrying out vortex mixing for 5-15 min, carrying out ultrasonic extraction for 5-15 min, filtering through a 0.22 mu m filter membrane, and carrying out sample injection to detect chloroacetic acid in the sample;
step (2), detection conditions: detecting chloroacetic acid by using an ultra performance liquid chromatography-tandem mass spectrometry UPLC-MS/MS as a detection instrument.
In the step (1), 0.185g of the product to be detected is taken, the precision is 0.01mg, the product is placed in an empty volumetric flask, acetonitrile-water 9:1 is added, the volume is fixed to 20ml, vortex mixing is carried out for 15min, ultrasonic extraction is carried out for 5min, and the mixture is filtered 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 a mass-to-charge ratio m/z of 93 → 93 and m/z of 93 → 77 are selected as a qualitative and quantitative ion pair; the chromatographic column of the ultra-high performance liquid chromatography-tandem mass spectrometry instrument is NH2High performance liquid chromatography column with bonded silica gel as stationary phase: the length of an amino column is 150mm, the diameter of the column is 4.6mm, and the grain diameter of the filler is 3.5 mu m; the flow rate of the ultra-high performance liquid chromatography-tandem mass spectrometry instrument is 0.4 ml/ml; the column temperature of the ultra-high performance liquid chromatography-tandem mass spectrometry instrument is 30 ℃; ultra-high performance liquid chromatography-clusterThe sample injection volume of the combined mass spectrometer is 5 mu L; the mass spectrum condition of the ultra-high performance liquid chromatography-tandem mass spectrometer is an HESI ion source, the capillary voltage is 2800-3800 v, the capillary temperature is 250-380 ℃, the ion source temperature is 130-250 ℃, the atomizing gas is nitrogen, the sheath gas pressure is 40psi, the auxiliary gas pressure is 5psi, the ion transmission voltage is-40 to-90 v, the collision gas is argon, the collision gas pressure is 1.0-2.0 mtorr, the collision energy is-5 to-20 v respectively, 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 fig. 1-2, about 185mg of chloroacetic acid standard was weighed into a 10ml volumetric flask, dissolved with acetonitrile-water 9:1 and brought to volume. Diluting the chloroacetic acid standard solution to 227ng/mL by using acetonitrile-water 9:1, and then taking 1.5mL to be injected into a sample injection vial for analysis to obtain a chloroacetic acid standard chromatogram. As shown in fig. 3 to 4, are chromatograms of acetonitrile-water 9:1 solvent. 1ml acetonitrile-water 9:1 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 183mg of rivaroxaban solid powder is respectively weighed into a 20ml volumetric flask, an appropriate amount of acetonitrile-water 9:1 is added, vortex mixing is carried out for 15min, ultrasonic extraction is carried out for 5min, volume is determined to be a scale by acetonitrile-water 9:1, 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 a chloroacetic acid standard chromatogram to see that the blank solvent of 9:1 acetonitrile-water and the blank matrix of the sample have no interference peak at the target peak position for 2.5-3.5 min; thus, it is believed that the solvent and sample matrix do not interfere with the chloroacetic acid detection.
Linear experiments:
as shown in FIG. 11, FIG. 13, FIG. 15, FIG. 17 and FIG. 19, about 185mg of chloroacetic acid standard is weighed into a 10ml volumetric flask, dissolved with 9:1 acetonitrile-water and fixed to the scale. Diluting the chloroacetic acid standard solution with acetonitrile-water 9:1 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 chloroacetic acid instrument shows a good linear relation in 227 ng/mL-911 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 spectrogram of the 91ng/mL chloroacetic acid standard substance; the signal-to-noise ratio of the detection signal reaches 20 and meets the detection limit requirement of S/N >3 at 2.5-3.5 min. 227ng/mL chloroacetic acid standard chromatogram and mass spectrum; the signal-to-noise ratio of the method reaches the quantitative limit requirement of S/N >10 when the signal-to-noise ratio is 50 at 2.5-3.5 min.
Precision:
a chloroacetic acid concentration point is selected for 6 times of repeated experiments, and 455ng/mL is selected as the concentration of the chloroacetic acid standard solution for precision experiments. The specific data are shown in the following table 2, and the table 2 is the precision experimental data of chloroacetic acid:
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: 24.8mg/kg, 49.7mg/kg, 74.6mg/kg, i.e., 227ng/mL, 455ng/mL, 683 ng/mL. The experimental data are shown in table 3 below, and table 3 is the chloroacetic acid standard recovery experimental data.
TABLE 3
As shown in Table 3, the experimental data of the standard recovery of chloroacetic acid can be seen, the recovery rate is 80-120%, and the experimental requirements are met.
Example 2
Example 2 differs from example 1 in that: adding acetonitrile-water 8:1 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 chloroacetic acid in a sample; taking the sample to be tested to 0.229g, accurately measuring to 0.01mg, placing in an empty volumetric flask, adding acetonitrile-water 8:1, diluting to 25ml, vortex mixing for 10min, and ultrasonic extracting for 6 min.
Example 3
Example 3 differs from example 1 in that: adding acetonitrile-water 6:1 to 50ml in the step (1), 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 chloroacetic acid in the sample; taking 0.458g of the sample to be detected, accurately measuring to 0.01mg, placing in an empty volumetric flask, adding acetonitrile-water 6:1, diluting to 50ml, mixing by vortex for 10min, and performing 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 chloroacetic acid 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 in a ratio of 1: 1-9: 1 to a constant volume of 10-50 ml, carrying out vortex mixing for 5-15 min, carrying out ultrasonic extraction for 5-15 min, filtering through a 0.22 mu m filter membrane, and carrying out sample injection to detect chloroacetic acid in the sample;
and (2) detecting chloroacetic acid by using an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) as a detection instrument.
2. The method for detecting chloroacetic acid by ultra high performance liquid chromatography-tandem mass spectrometry according to claim 1, wherein: 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 93 → 93 and a mass-to-charge ratio m/z 93 → 77 as a qualitative and quantitative ion pair.
3. The method for detecting chloroacetic acid by ultra high performance liquid chromatography-tandem mass spectrometry according to claim 1, wherein: in the step (2), the chromatographic column of the ultra-high performance liquid chromatography-tandem mass spectrometer is-NH2High performance liquid chromatography column with bonded silica gel as 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 3.5 mu m.
4. The method for detecting chloroacetic acid by ultra high performance liquid chromatography-tandem mass spectrometry according to 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/ml.
5. The method for detecting chloroacetic acid by ultra high performance liquid chromatography-tandem mass spectrometry according to claim 1, wherein: in the step (2), the column temperature of the ultra-high performance liquid chromatography-tandem mass spectrometry instrument is 25-45 ℃.
6. The method for detecting chloroacetic acid by ultra high performance liquid chromatography-tandem mass spectrometry according to claim 1, wherein: in the step (2), the sample injection volume of the ultra-high performance liquid chromatography-tandem mass spectrometry instrument is 2-20 mu L.
7. The method for detecting chloroacetic acid by ultra high performance liquid chromatography-tandem mass spectrometry according to claim 1, wherein: in the step (2), the mass spectrum condition of the ultra-high performance liquid chromatography-tandem mass spectrometer is an HESI ion source, the capillary tube voltage is 2800-3800 v, the capillary tube temperature is 250-380 ℃, the ion source temperature is 130-250 ℃, 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 to-90 v, the collision gas is argon, the collision gas pressure is 1.0-2.0 mtorr, the collision energy is respectively-5 v to-30 v, and the scanning time is 0.1-1.0 second.
8. The method for detecting chloroacetic acid by ultra high performance liquid chromatography-tandem mass spectrometry according to claim 1, wherein: in the step (1), the sample to be detected is 0.1-0.5 g, and the accuracy is 0.01 mg.
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Cited By (1)
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| CN115290792A (en) * | 2022-08-04 | 2022-11-04 | 英格尔检测技术服务（上海）有限公司 | Liquid chromatography-mass spectrometry combined detection method for chloroacetic acid residues in bulk drugs |
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| CN102520083A (en) * | 2011-12-05 | 2012-06-27 | 西安建筑科技大学 | Method for quickly detecting haloacetic acids serving as disinfection byproducts in drinking water |
| CN107422053A (en) * | 2017-07-04 | 2017-12-01 | 苏州出入境检验检疫局检验检疫综合技术中心 | A kind of method of trichloroacetic acid in LC-MS detection cosmetics |
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| CN102520083A (en) * | 2011-12-05 | 2012-06-27 | 西安建筑科技大学 | Method for quickly detecting haloacetic acids serving as disinfection byproducts in drinking water |
| CN107422053A (en) * | 2017-07-04 | 2017-12-01 | 苏州出入境检验检疫局检验检疫综合技术中心 | A kind of method of trichloroacetic acid in LC-MS detection cosmetics |
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| CN115290792A (en) * | 2022-08-04 | 2022-11-04 | 英格尔检测技术服务（上海）有限公司 | Liquid chromatography-mass spectrometry combined detection method for chloroacetic acid residues in bulk drugs |
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