CN111679007A - Method for simultaneously detecting 13 halogenated amide disinfection byproducts in drinking water - Google Patents
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Abstract
The invention relates to a method for simultaneously detecting 13 halogenated amide (HAcAms) disinfection byproducts in drinking water, belonging to the field of analytical chemistry. The method aims to provide the method for simultaneously measuring 13 halogenated amides in the drinking water without enriching and concentrating the sample, improve the analysis efficiency and avoid the use of an organic solvent in the pretreatment process and the health influence on operators. The method adopts the high performance liquid chromatography-tandem mass spectrometer for determination, determines detailed instrument parameter conditions, only needs 10 minutes for detecting one sample, adopts an automatic sample injector for sample injection, can realize high flux accurate quantification of the sample, has high standard adding recovery rate and high detection sensitivity, can achieve concentration detection of ng/L level by direct sample injection, and is favorable for promoting development of HAcAms monitoring work of drinking water.
Description
Technical Field
The invention belongs to the field of health detection, relates to a water quality detection and analysis technology, and particularly relates to a method for simultaneously detecting 13 halogenated amide disinfection byproducts in drinking water by using a high performance liquid chromatography-tandem mass spectrometer;
background
Drinking water disinfection is widely popularized due to the capability of effectively controlling water-mediated infectious diseases caused by pathogenic microorganisms in water, and becomes one of the most important technical advances in the field of public health in the twentieth century; however, the drinking water is disinfected just like a 'double-edged sword', and the drinking water disinfects pathogenic microorganisms in water and brings the health hazard problem of disinfection byproducts in the drinking water;
in 1974, Rook and Beller et al first discovered chloroform (CHCl) in chlorinated, disinfected drinking water3) Trihalomethanes (THMs) representative of disinfection by-products; in 1976, results of national surveys conducted by the U.S. environmental protection agency (u.s.epa) showed the ubiquitous presence of THMs in chlorinated, disinfected drinking water; in the same year, the National Cancer Institute (NCI) reported CHCl3Can cause renal tubular cell adenocarcinoma of male rat and hepatocellular carcinoma of female mouse; the subsequent salmonella typhimurium back mutation experiment (Ames) result shows that the organic extract of the drinking water has mutagenicity; the results of this series of studies have raised a great deal of attention to the major public health problem of drinking water disinfection by-products; to reduce the by-product of disinfection as much as possibleHealth risks brought to people, and disinfection byproducts such as THMs, Halogenated Acetic Acids (HAAs), bromate, chlorate, chlorite and the like are brought into relevant drinking water standards in sequence by a plurality of countries and organizations such as China, the United states, Japan, the World Health Organization (WHO), the European Union (EU) and the like according to relevant research results, and corresponding standard limit values are formulated; however, the types and contents of disinfection byproducts in drinking water vary with the types of disinfectants used in disinfection processes and the water pollution conditions of water sources, and with the rapid development of detection technologies, more than 700 DBPs are found in drinking water and disinfection simulation experiments; in 2006-2007, large-scale investigation on pollution conditions of drinking water disinfection byproducts is carried out, systematic investigation is carried out on more than 70 new disinfection byproducts including nitrogen-containing disinfection byproducts such as Haloacetonitrile (HANs) and Halogenated Nitromethane (HNMs), and halogenated amide (HAcAms) disinfection byproducts are found for the first time;
HAcAms refers to a substance formed by replacing hydrogen on acetamide by halogen, and hydrogen on a carbon atom directly connected with acetyl is replaced by chlorine, bromine and iodine respectively to form monohaloamide, dihaloamide and trihaloamide; there are 13 HAcAms reported so far, and the chemical structure and basic information are shown in fig. 1 and table 1; relevant toxicity research data show that the toxicity of HAcAms is obviously higher than that of conventional disinfection byproducts such as THMs, HAAs and the like controlled by drinking water relevant standards; the investigation result of national researchers in the United states, Australia, Japan, UK and the like on the HAcAms pollution condition of drinking water in partial regions shows that partial HAcAms are detected, and the maximum total concentration of the HAcAms is (3.80-8.18) mu g/L; the concentration range of part of HAcAms in Shenzhen drinking water in China is (0.1-3.1) mu g/L, but the HAcAms pollution condition of the drinking water is still lack of system understanding due to the limit value of the detection limit of the existing detection method; these unique properties present major difficulties in the detection of HAcAms in drinking water, since the binding between hydrogen and adjacent amide groups in the HAcAms structure is very strong, and although they are of low molecular mass, they are not volatile and are susceptible to hydrolysis under acidic and basic conditions; at present, the reported detection methods mainly include gas chromatography (GC-ECD), gas chromatography-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (LC-MS), and the like, and the existing methods all need to combine liquid-liquid extraction (LLE), solid-phase extraction (SPE), acid-catalyzed hydrolysis, silanization and other pretreatment; on the one hand, the pretreatment process is complex and needs a large amount of manpower, material resources and time, on the other hand, the pretreatment process cannot recover 100 percent of HAcAms in a drinking water sample, and the HAcAms can be hydrolyzed in the process, so that the haloamide in the drinking water is difficult to detect or the detected concentration is low; in addition, the sensitivity of these methods cannot meet the detection requirement of lower concentration HAcAms in drinking water; the above limitations of the existing detection methods limit the development of HAcAms monitoring work in drinking water; as shown in fig. 1 and table 1:
table 113 HAcAms basic information
Chinese patent CN106596751A discloses a high performance liquid chromatography # electrospray mass spectrometry detection method for chloro-disinfection byproducts dichloroacetamide and trichloroacetamide, CN105866287A and CN106338559B disclose a gas chromatography detection method for chloro-disinfection byproducts dichloroacetamide, both of which have the advantages of simplicity, high efficiency, high sensitivity, wide linear range, good reproducibility, high recovery rate, accurate instrument analysis result, clear spectrogram analysis and the like, but only can simultaneously detect two HAcAms of dichloroacetamide and trichloroacetamide or detect dichloroacetamide alone, and cannot realize simultaneous detection of 13 HAcAms; in addition, the two methods also need to adopt solid phase extraction or liquid-liquid extraction to concentrate and enrich the sample;
disclosure of Invention
The invention aims to provide a method for simultaneously detecting 13 halogenated amide disinfection byproducts in drinking water, which overcomes the defects of the prior method in aspects of sample pretreatment, recovery rate, sensitivity and the like, can realize high-flux detection of low ng/L concentration HAcAms in the drinking water by directly feeding samples on the premise of no need of enrichment and concentration, can realize quick positive and negative switching without losing sensitivity, has strong pollution resistance, can feed samples after a drinking water sample is simply centrifuged to remove impurities, and ensures the accuracy of results;
the purpose of the invention can be realized by the following technical scheme:
operating parameters of high performance liquid chromatography-tandem mass spectrometer
1. Chromatographic conditions
The chromatographic column is HSS T3,2.5 μm,2.1 × 150 mm; the mobile phase comprises a mobile phase A and a mobile phase B: the mobile phase A is 0.1 percent acetic acid water, the mobile phase B is acetonitrile, and the concentration is 0.4 mL/min; gradient elution was used: mobile phase A + mobile phase B is 100%; the volume percentage of the mobile phase A is reduced from 95% to 60% in 0-7 min; 7-8 min, and keeping the volume percentage of the mobile phase A at 60%; 8.1-10 min, and keeping the volume percentage of the mobile phase A at 95%; the column temperature is 40 min; the sample injection amount is 50 mu L; the flow rate is 0.4 mL/min;
2. conditions of Mass Spectrometry
ESI source, mass spectrometric multiple reaction monitoring mode (MRM), air Curtain Gas (CUR) 30psi, collisional Gas (colloid Gas) medium, Ion Spray Voltage (IS) 5500/-4500V, Ion source Temperature (TEM) 400 ℃, nebulizing Gas (Nebulizer Gas, GS1)55psi, drying Gas (Heater Gas, GS2)55 psi;
the triple quadrupole mass spectrometer was manufactured as AB SCIEX model Qtrap 6500+；
3. Determination of Mass Spectrometry parameters of 13 HAcAms
The 13 HAcAms and the mass spectrum parameters thereof are shown in Table 2
TABLE 2
Second, sample detection and analysis
1. Drawing a standard curve of 13 HAcAms
(1) Preparing standard solution
The 13 HAcAms are commercially available, wherein CAcAm (≧ 98.0%), BAcAm (98%), IAcAm (≧ 99.0%), TCAcAm (99.0%) was purchased from Sigma-Aldrich, usa, BCAcAm (99 +%), BDCAcAm (99 +%), TBAcAm (99 +%), ciam (99 +%), DBAcAm (99 +%), DIAcAm (99 +%) and BIAcAm (85 +%) were purchased from canada CanSyn Chem, DCAcAm (98 +%) was purchased from shanghai warfarin (J & kchemial Ltd.); respectively weighing appropriate amount of 13 HAcAms standard substances, and preparing into single standard stock solution with concentration of 1000mg/L with methanol; respectively taking 50 mul of 13 HAcAms single-standard stock solutions, mixing, and then using ultrapure water to perform constant volume to 5ml to obtain a mixed standard stock solution with the concentration of 10mg/L, and then using ultrapure water to perform dilution before use to obtain a HAcAms mixed standard use solution with the concentration of 1 mg/L; then respectively sucking a certain volume of mixed standard, diluting with ultrapure water to obtain standard series solutions with the concentrations of 0.001 mu g/L, 0.005 mu g/L, 0.010 mu g/L, 0.025 mu g/L, 0.050 mu g/L, 0.100 mu g/L, 0.200 mu g/L, 0.300 mu g/L, 0.500 mu g/L, 1.00 mu g/L, 5.00 mu g/L, 10.0 mu g/L and 100 mu g/L respectively, storing the standard stock solutions in brown bottles, and placing in a refrigerator for dark preservation at 4 ℃;
(2) analyzing the standard solutions with different concentrations by adopting a high performance liquid chromatography-tandem mass spectrometer, and determining according to the parameters determined in the step one to obtain chromatograms of 13 HAcAms in the standard solutions; obtaining the retention time, the area of a quantitative ion pair and the area of a qualitative ion pair of each HAcAm in the standard solution from the chromatogram; taking the area of each HAcAm quantitative ion pair in the standard solution as a vertical coordinate and the concentration of each HAcAm in the standard solution as a horizontal coordinate to obtain standard curves of 13 HAcAms standard products;
2. centrifuging 10mL of the drinking water sample at 10000rpm for 5min, then placing 1mL of the drinking water sample into a sample feeding bottle, injecting the drinking water sample into a high performance liquid chromatography-tandem mass spectrometer through an autosampler of the high performance liquid chromatography-tandem mass spectrometer, and determining according to the parameters determined in the first step to obtain a chromatogram of the drinking water sample;
3. obtaining the retention time, the area of a quantitative ion pair and the area of a qualitative ion pair of each HAcAm in the drinking water sample from the chromatogram of the drinking water sample obtained in the step 2; and (3) comparing the retention time of each HAcAm in the drinking water sample, the area ratio of the qualitative ion pair to the quantitative ion pair with the retention time of each HAcAm in the standard solution obtained in the step two-1- (2), and the area ratio of the qualitative ion pair to the quantitative ion pair, qualitatively analyzing 13 HAcAms in the drinking water sample, and quantitatively analyzing the drinking water sample according to the standard curve of the 13 HAcAms standard products obtained in the step two-1- (2) to obtain the content of 13 HAcAms in the drinking water sample.
The invention has the following beneficial effects:
1. the method adopts direct sample introduction, avoids a complicated sample pretreatment process, reduces the HAcAms loss of the sample, and avoids the use of an organic solvent in the pretreatment process and the health influence on operators;
2. the method adopts the high performance liquid chromatography-tandem mass spectrometer for determination, only 10 minutes are needed for detecting one sample, the high-flux accurate quantification of the sample can be realized, the detection sensitivity is high, the concentration detection of ng/L level can be achieved without enrichment and concentration, the method has extremely strong anti-pollution capacity, and the drinking water sample can be injected by simply centrifuging at high speed and taking supernatant; the detection sensitivity is expressed by detection limit, and the detection limit of 13 HAcAms in the method is 0.001-0.1 mug/L; the linear relation of the standard curve is good, and the correlation coefficients are all larger than 0.995; performing a labeling recovery experiment by using ultrapure water as a blank background, wherein the labeling recovery rate of 3 concentrations of 0.5 mug/L, 1.0 mug/L and 5.0 mug/L is 70-120%;
3. the method can simultaneously determine 13 HAcAms of drinking water, avoids complicated sample pretreatment process on the basis of the existing method, expands the detection range of only detecting one or two HAcAms, and obviously improves the analysis efficiency;
4. the invention adopts the automatic sample injector for sample injection, does not need to be attended by personnel, and can automatically complete the measurement of a large batch of samples.
Drawings
FIG. 113 chemical structures of HAcAms,
FIG. 213 chromatogram of HAcAms,
fig. 3 chloroacetamide y 2.12117e5x +12846.77511(r2 0.994),
figure 4 bromoacetamide y ═ 4.19577e5x + -788.51358(r2 ═ 0.993),
figure 5 monochloromonobromoacetamide y ═ 4.12422e5x +1474.15556(r2 ═ 0.997),
figure 6 iodoacetamide y-1.10107 e6x +263.67969(r 2-0.997),
figure 7 dibromoacetamide y-3.51105 e4x +1523.31214(r 2-0.994),
figure 8 monochloromonodoacetamide y-1.36186 e6x +21061.58208(r 2-0.997),
figure 9 monobromonoiodoacetamide y ═ 7.96555e5x + -3115.58268(r2 ═ 0.999),
figure 10 tribromoacetamide y-9.46847 e4x +18521.80758(r 2-0.994),
figure 11 diiodoacetamide y 2.83739e6x +9719.94511(r2 0.998),
in figure 12, dichloroacetamide, y is 3.48758e4x +7637.32717(r2 is 0.994),
figure 13 trichloroacetamide y-4.11098 e4x +5601.84904(r 2-0.999),
figure 14 dichloro monobromoacetamide y-16334.32286 x +793.18113(r 2-0.997),
fig. 15 monochloro dibromoacetamide y-20137.13833 x +398.01775(r 2-0.994).
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
the embodiment detects the factory water and the peripheral water; the method for simultaneously detecting 13 halogenated amide disinfection byproducts in drinking water by adopting the high performance liquid chromatography-tandem mass spectrometer is carried out according to the following steps:
operating parameters of high performance liquid chromatography-tandem mass spectrometer
1. Chromatographic conditions
The chromatographic column is HSS T3,2.5 μm,2.1 × 150 mm; the mobile phase comprises a mobile phase A and a mobile phase B: the mobile phase A is 0.1 percent acetic acid water, the mobile phase B is acetonitrile, and the concentration is 0.4 mL/min; gradient elution was used: mobile phase A + mobile phase B is 100%; the volume percentage of the mobile phase A is reduced from 95% to 60% in 0-7 min; 7-8 min, and keeping the volume percentage of the mobile phase A at 60%; 8.1-10 min, and keeping the volume percentage of the mobile phase A at 95%; the column temperature is 40 min; the sample injection amount is 50 mu L; the flow rate is 0.4 mL/min;
2. conditions of Mass Spectrometry
ESI source, mass spectrometric multiple reaction monitoring mode (MRM), air Curtain Gas (CUR) 30psi, collisional Gas (colloid Gas) medium, Ion Spray Voltage (IS) 5500/-4500V, Ion source Temperature (TEM) 400 ℃, nebulizing Gas (Nebulizer Gas, GS1)55psi, drying Gas (Heater Gas, GS2)55 psi;
the triple quadrupole mass spectrometer was manufactured as AB SCIEX model Qtrap 6500+；
3. Determination of Mass Spectrometry parameters of 13 HAcAms
The 13 HAcAms and their mass spectrum parameters are shown in table 3;
TABLE 313 Haloamide Mass Spectrometry parameters
Second, sample detection and analysis
1. Drawing a standard curve of 13 HAcAms
(1) Preparing standard solution
The 13 HAcAms are commercially available, wherein CAcAm (≧ 98.0%), BAcAm (98%), IAcAm (≧ 99.0%), TCAcAm (99.0%) was purchased from Sigma-Aldrich, usa, BCAcAm (99 +%), BDCAcAm (99 +%), TBAcAm (99 +%), ciam (99 +%), DBAcAm (99 +%), DIAcAm (99 +%) and BIAcAm (85 +%) were purchased from canada CanSyn Chem, DCAcAm (98 +%) was purchased from shanghai warfarin (J & kchemial Ltd.); respectively weighing appropriate amount of 13 HAcAms standard substances, and preparing into single standard stock solution with concentration of 1000mg/L with methanol; respectively taking 50 mul of 13 HAcAms single-standard stock solutions, mixing, and then using ultrapure water to perform constant volume to 5ml to obtain a mixed standard stock solution with the concentration of 10mg/L, and then using ultrapure water to perform dilution before use to obtain a HAcAms mixed standard use solution with the concentration of 1 mg/L; then respectively sucking a certain volume of mixed standard, diluting with ultrapure water to obtain standard series solutions with the concentrations of 0.001 mu g/L, 0.005 mu g/L, 0.010 mu g/L, 0.025 mu g/L, 0.050 mu g/L, 0.100 mu g/L, 0.200 mu g/L, 0.300 mu g/L, 0.500 mu g/L, 1.00 mu g/L, 5.00 mu g/L, 10.0 mu g/L and 100 mu g/L respectively, storing the standard stock solutions in brown bottles, and placing in a refrigerator for dark preservation at 4 ℃;
(2) analyzing the standard solutions with different concentrations by using a high performance liquid chromatography-tandem mass spectrometer, and determining according to the parameters determined in the step one to obtain chromatograms of 13 HAcAms in the standard solutions (as shown in figure 2); obtaining the retention time, the area of a quantitative ion pair and the area of a qualitative ion pair of each HAcAm in the standard solution from the chromatogram; taking the area of each HAcAm quantitative ion pair in the standard solution as a vertical coordinate and the concentration of each HAcAm in the standard solution as a horizontal coordinate to obtain standard curves of 13 HAcAms standard products;
taking the concentration of each HAcAm in the standard solution as a horizontal coordinate to obtain standard curves of 13 HAcAms standard products; the standard curves for the 13 HAcAms standards are shown in fig. 3-15:
(3) method detection limit
The detection limits of 13 HAcAms are shown in table 3;
table 313 HAcAms detection limits
| HAcAms | Detection Limit concentration (μ g/L) | HAcAms | Detection Limit concentration (μ g/L) |
| Chloroacetamides | 0.001 | Monochloro-iodoacetamide | 0.005 |
| Dichloroacetamide | 0.005 | Monobromonoiodoacetamide | 0.010 |
| Bromoacetamide | 0.050 | Tribromoacetamide | 0.100 |
| Trichloroacetamide | 0.100 | Diiodoacetamide | 0.001 |
| Monochloro-monobromoacetamide | 0.050 | Dichloro-monobromoacetamide | 0.100 |
| Iodoacetamide | 0.005 | Monochloro dibromo acetamide | 0.050 |
| Dibromoacetamide | 0.100 |
(4) Recovery by adding a label
Taking ultrapure water as a blank background, respectively adding a certain volume of mixed standard solution to prepare water samples with the concentrations of 0.50, 1.00 and 5.00 mu g/L, and investigating the reliability of the method, wherein the results are shown in Table 4;
table 413 HAcAms standard adding and recycling conditions
The 13 HAcAms obtained in the embodiment has good linearity (r is more than 0.995), the lowest detection limit can be up to 1ng/L, the recovery rate is between 70 and 120 percent, and the detection result has high accuracy;
2. centrifuging 10mL of the drinking water sample at 10000rpm for 5min, then placing 1mL of the drinking water sample into a sample feeding bottle, injecting the drinking water sample into a high performance liquid chromatography-tandem mass spectrometer through an autosampler of the high performance liquid chromatography-tandem mass spectrometer, and determining according to the parameters determined in the first step to obtain a chromatogram of the drinking water sample;
3. obtaining the retention time, the area of a quantitative ion pair and the area of a qualitative ion pair of each HAcAm in the drinking water sample from the chromatogram of the drinking water sample obtained in the step 2; comparing the retention time of each HAcAm in the drinking water sample, the area ratio of the qualitative ion pair to the quantitative ion pair with the retention time of each HAcAm in the standard solution obtained in the step two-1- (2), and the area ratio of the qualitative ion pair to the quantitative ion pair, qualitatively analyzing 13 HAcAms in the drinking water sample, and quantitatively analyzing 13 HAcAms in the drinking water sample according to the standard curve of the 13 HAcAms standard products obtained in the step two-1- (2) to obtain the content of 13 HAcAms in the drinking water sample;
the detection results of this example are shown in Table 5;
TABLE 5 HAcAms assay results (μ g/L) for 13 of the drinking water samples
Claims (1)
1. A method for simultaneously detecting 13 halogenated amide disinfection byproducts in drinking water is characterized by comprising the following steps:
1) operating parameters of the high performance liquid chromatography-tandem mass spectrometer,
1, chromatographic conditions
The chromatographic column is HSS T3,2.5 μm,2.1 × 150 mm; the mobile phase comprises a mobile phase A and a mobile phase B: the mobile phase A is 0.1 percent acetic acid water, the mobile phase B is acetonitrile, and the concentration is 0.4 mL/min; gradient elution was used: mobile phase A + mobile phase B is 100%; the volume percentage of the mobile phase A is reduced from 95% to 60% in 0-7 min; 7-8 min, and keeping the volume percentage of the mobile phase A at 60%; 8.1-10 min, and keeping the volume percentage of the mobile phase A at 95%; the column temperature is 40 min; the sample injection amount is 50 mu L; the flow rate is 0.4 mL/min;
2, Mass Spectrometry Condition
ESI source, mass spectrum multiple reaction monitoring mode, gas curtain gas 30psi, collision gas medium, ion spray voltage 5500/-4500V, ion source temperature 400 ℃, atomizing gas 55psi, drying gas 55 psi; the triple quadrupole mass spectrometer was manufactured as AB SCIEX model Qtrap 6500+；
3, according to the following table, the mass spectrometric parameters of 13 HAcAms were determined,
2) sample detection and analysis
1, drawing the standard curve of 13 HAcAms
(1) Preparing standard solution
The 13 HAcAms are commercially available products, wherein CAcAm is more than or equal to 98.0%, BAcAm 98%, IAcAm is more than or equal to 99.0%, TCAcAm 99.0% is purchased from Sigma-Aldrich, USA, BCAcAm 99 +%, BDACAm 99 +%, TBAcAm 99 +%, CIAcAm 99 +%, DBCAcAm 99 +%, DBAcAm 99 +%, DIAcAm 99 +% and BIAcAm 85 +%, DCAcAm98 +%; respectively weighing appropriate amount of 13 HAcAms standard substances, and preparing into single standard stock solution with concentration of 1000mg/L with methanol; respectively taking 50 mul of 13 HAcAms single-standard stock solutions, mixing, and then using ultrapure water to perform constant volume to 5ml to obtain a mixed standard stock solution with the concentration of 10mg/L, and then using ultrapure water to perform dilution before use to obtain a HAcAms mixed standard use solution with the concentration of 1 mg/L; then respectively sucking a certain volume of mixed standard, diluting with ultrapure water to obtain standard series solutions with the concentrations of 0.001 mu g/L, 0.005 mu g/L, 0.010 mu g/L, 0.025 mu g/L, 0.050 mu g/L, 0.100 mu g/L, 0.200 mu g/L, 0.300 mu g/L, 0.500 mu g/L, 1.00 mu g/L, 5.00 mu g/L, 10.0 mu g/L and 100 mu g/L respectively, storing the standard stock solutions in brown bottles, and placing in a refrigerator for dark preservation at 4 ℃;
(2) analyzing the standard solutions with different concentrations by adopting a high performance liquid chromatography-tandem mass spectrometer, and determining according to the parameters determined in the step one to obtain chromatograms of 13 HAcAms in the standard solutions; obtaining the retention time, the area of a quantitative ion pair and the area of a qualitative ion pair of each HAcAm in the standard solution from the chromatogram; taking the area of each HAcAm quantitative ion pair in the standard solution as a vertical coordinate and the concentration of each HAcAm in the standard solution as a horizontal coordinate to obtain standard curves of 13 HAcAms standard products;
2, centrifuging 10mL of the drinking water sample at 10000rpm for 5min, then placing 1mL of the drinking water sample into a sample injection bottle, injecting the drinking water sample into a high performance liquid chromatography-tandem mass spectrometer through an automatic sample injector of the high performance liquid chromatography-tandem mass spectrometer, and determining according to the parameters determined in the step one to obtain a chromatogram of the drinking water sample;
3, obtaining the retention time, the area of a quantitative ion pair and the area of a qualitative ion pair of each HAcAm in the drinking water sample from the chromatogram of the drinking water sample obtained in the step 2; comparing the retention time of each HAcAm in the drinking water sample, the area ratio of the qualitative ion pair to the quantitative ion pair with the retention time of each HAcAm in the standard solution obtained in the step 2) -1- (2), and the area ratio of the qualitative ion pair to the quantitative ion pair, qualitatively analyzing 13 HAcAms in the drinking water sample, and quantitatively analyzing the drinking water sample according to the standard curves of the 13 HAcAms standard products obtained in the step 2) -1- (2), so as to obtain the content of 13 HAcAms in the drinking water sample.
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| CN112763612A (en) * | 2020-12-28 | 2021-05-07 | 北京诺康达医药科技股份有限公司 | Detection method of halogenated amide substances |
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