KR101936848B1 - A method for determination of ethylene oxide in foodstuff using derivatization - Google Patents

Abstract

The present invention can perform accurate analysis with lower detection limit by converting ethylene oxide contained in a sample to be analyzed such as food into 2-chloroethanol and reacting the derivative after the reaction. Also, the present invention can simultaneously analyze ethylene oxide and 2-chloroethanol as a decomposition product thereof.

Description

[0001] The present invention relates to a method for the determination of ethylene oxide in foods using a derivative,

Disclosed herein is an analytical method for accurately measuring the amount of ethylene oxide in a sample.

Ethylene oxide is the easiest epoxide. It has high reactivity, so it is used as an intermediate material when producing chemical substances. It has strong sterilizing power and insecticidal power, so it can be used as an industrial detergent, It is widely used for the production of active agents, fumigant for agricultural chemicals, medical and food sterilizing chemicals.

However, ethylene oxide has strong toxicity, and the International Agency for Research on Cancer (IARC) has classified ethylene oxide as a human carcinogenic substance, GROUP 1. Residual ethylene oxide reacts with various compounds to react with glycols and salt to produce chlorhydrin, respectively. For this reason, it is totally prohibited to use ethylene oxide in food processing in Korea at present, but it is still used as a bactericide and pesticide fumigant for packaging products and has high persistence, so ethylene oxide can be detected in food, and continuous monitoring is required .

Therefore, there is a need for a method that can more accurately and accurately analyze ethylene oxide in food samples.

Conventional methods for detecting and analyzing ethylene oxide include various extraction methods such as head space method and SPME (Solid Phase Micro Extraction) method. A device analysis using a capillary column as disclosed in JP 2001-021545 A shows that since the acetaldehyde and the retention time are the same in the polarity column and the molecular ion and the quantitative ion are the same, the ethylene oxide and the acetaldehyde are not separated, There is a problem that accurate detection and quantification can not be performed.

In the spices disclosed in F. Tateo et al. (Determination of ethylene chlorohydrin as a marker of spices fumigation with ethylene oxide, F. Tateo, M. Bononi, Journal of Food Composition and Analysis, 2006, vol 19, p83-87) The method of measuring the concentration of chloroethanol and using it as a marker of whether ethylene oxide is fumigated has a problem that accuracy can not be guaranteed since 2-chloroethanol can not be regarded as being derived from 100% ethylene oxide.

JP 2001-021545 A JP 1982-149961 A

Determination of ethylene chlorohydrin as marker of spices fumigation with ethylene oxide, F. Tateo, M. Bononi, Journal of Food Composition and Analysis, 2006, vol 19, p83-87

In one aspect, an object of the present invention is to provide a method for accurately detecting and quantifying ethylene oxide.

In order to accomplish the above object, an embodiment of the present invention provides a method for separating a sample, comprising: an acid decomposition step of heating an analyte under acidic conditions to convert ethylene oxide contained in the sample into 2-chloroethanol;

A derivatization step of reacting the acid-decomposed sample with a derivative reagent;

Measuring the concentration of the derivatized 2-chloroethanol in the derivatized sample; And

Analyzing the amount of ethylene oxide contained in the sample to be analyzed by calculating the amount of conversion of the ethylene oxide to 2-chloroethanol from the concentration of the derivatized 2-chloroethanol measured from the sample;

And a method for quantitative analysis of ethylene oxide.

In addition, one embodiment of the present invention includes an acid decomposition step of heating a sample to be analyzed under acidic conditions to convert ethylene oxide contained in the sample into 2-chloroethanol;

A derivatization step of reacting the acid-decomposed sample with a derivative reagent;

Measuring the concentration of the derivatized 2-chloroethanol in the derivatized sample;

Calculating the amount of conversion of said ethylene oxide to 2-chloroethanol from the concentration of the derivatized 2-chloroethanol measured from said sample; And

Determining that ethylene oxide in the sample to be analyzed is included if the conversion amount is greater than 0;

And a method for detecting ethylene oxide.

Another embodiment of the present invention relates to a reaction apparatus comprising an acid, a salt and a heating device for converting ethylene oxide to 2-chloroethanol; A derivative reagent of 2-chloroethanol and a mass spectrometer, or a kit for quantitative analysis of ethylene oxide.

The present invention can conduct accurate analysis with lower detection limit of about 1.6 ppb by converting ethylene oxide contained in a sample to be analyzed such as foods into 2-chloroethanol and conducting the analysis. Since the present invention converts ethylene oxide to 2-chloroethanol, ethylene oxide, retention time, molecular ion, and quantitative ion can be analyzed without being interrupted by the same acetaldehyde. This solves the problem that conventional acetaldehyde and ethylene oxide are overlapped in a polarity column. In addition, by introducing a derivative reaction, excellent detection and quantitative sensitivity can be provided.

In addition, ethylene oxide may be spontaneously decomposed into 2-chloroethanol, ethylene glycol, or the like in foods. The present invention is a method of measuring and comparing accurate and inexpensive samples of ethylene oxide with 2-chloroethanol And quantification is possible. Therefore, the accuracy was improved compared with the method of estimating the concentration of ethylene oxide only by measuring the concentration of 2-chloroethanol. In addition, ethylene oxide and its decomposition product, 2-chloroethanol, can be simultaneously analyzed.

FIG. 1 is a view showing a route in which ethylene oxide is converted into 2-chloroethanol or ethylene glycol in the presence of an acid or a salt.
FIG. 2 is a graph showing the results of the reaction of 2-chloroethanol with N, O-bis- (trimethylsilyl) -trifluoroacetamide (BSTFA) and trimethyl chloro silane (Sigma-Aldrich, Steinheim, Germany) of 99: 1 (v / v) solution of TMCS.
3 is a graph showing the results of analysis of silylated 2-chloroethanol, i.e., (2-chloroethoxy) trimethylsilane, contained in the sample to be analyzed in Example 1, using a mass spectrometer. -chloroethoxy) trimethylsilane)
FIG. 4 is a view showing extraction methods according to Comparative Examples 1 and 2 which are conventional extraction methods. FIG.
5 is a diagram showing mass spectrometric conditions of Comparative Examples 1 and 2 which are conventional extraction methods.
6 is a view comparing the analysis results of Example 1 and Comparative Examples 1 and 2. FIG.

Hereinafter, the present invention will be described in detail.

One embodiment of the present invention provides a method for quantitative analysis of ethylene oxide or a method for detecting ethylene oxide.

In one embodiment, the method for quantitatively analyzing ethylene oxide comprises:

An acid decomposition step in which the sample to be analyzed is heated under acidic conditions to convert ethylene oxide contained in the sample to 2-chloroethanol;

A derivatization step of reacting the acid-decomposed sample with a derivative reagent;

Measuring the concentration of the derivatized 2-chloroethanol in the derivatized sample; And

And analyzing the amount of ethylene oxide contained in the sample to be analyzed by calculating the amount of conversion of the ethylene oxide to 2-chloroethanol from the concentration of the derivatized 2-chloroethanol measured from the sample .

In one embodiment, the method of detecting ethylene oxide comprises:

An acid decomposition step in which the sample to be analyzed is heated under acidic conditions to convert ethylene oxide contained in the sample to 2-chloroethanol;

A derivatization step of reacting the acid-decomposed sample with a derivative reagent;

Measuring the concentration of the derivatized 2-chloroethanol in the derivatized sample;

Calculating the amount of conversion of said ethylene oxide to 2-chloroethanol from the concentration of the derivatized 2-chloroethanol measured from said sample; And

And determining that the ethylene oxide in the sample to be analyzed is included if the conversion amount is greater than 0.

The quantitative analysis or detection method of ethylene oxide according to an embodiment of the present invention can separate ethylene oxide and acetaldehyde by converting ethylene oxide as an analyte into 2-chloroethanol under acidic conditions, You can provide a method.

Specifically, in the quantitative analysis method or the detection method of ethylene oxide according to an embodiment of the present invention, the amount of conversion of the ethylene oxide to 2-chloroethanol is calculated from the concentration of the derivatized 2-chloroethanol measured from the sample Step may include a step of derivatizing the sample to be analyzed without derivatizing ethylene oxide to 2-chloroethanol, and a step of measuring the concentration of the derivatized 2-chloroethanol in the derivatized sample.

And the concentration of the derivatized 2-chloroethanol measured from the sample in which the ethylene oxide is converted to 2-chloroethanol and the concentration of the derivatized 2-chloroethanol measured from the sample not converting the ethylene oxide into 2-chloroethanol Calculating the amount of conversion of ethylene oxide to 2-chloroethanol from the tea; As shown in FIG.

That is, the step according to one embodiment calculates the difference in 2-chloroethanol concentration between the sample not converted to ethylene oxide contained in the sample to be analyzed and the sample converted to 2-chloroethanol, To calculate the concentration of 2-chloroethanol converted from the oxide, that is, the amount of conversion to 2-chloroethanol, and thereby to calculate the concentration of ethylene oxide.

In the method for quantitative analysis or detection of ethylene oxide according to an embodiment of the present invention, the step of calculating the amount of conversion of ethylene oxide into 2-chloroethanol may include the step of converting the ethylene oxide into 2-chloroethanol To the concentration of 2-chloroethanol contained in the sample to be analyzed, excluding the calculated conversion amount of ethylene oxide into 2-chloroethanol at the concentration of the derivatized 2-chloroethanol measured from the concentration of 2-chloroethanol can do. Thus, according to an embodiment of the present invention, it is possible to simultaneously quantify ethylene oxide and 2-chloroethanol contained in the sample to be analyzed.

In the method for quantitative analysis or detection of ethylene oxide according to an embodiment of the present invention, the step of measuring the concentration of the derivatized 2-chloroethanol in the derivatized sample may include a measurement using a mass spectrometer, As long as the concentration of the derivatized 2-chloroethanol in the derivatized sample can be measured.

In the quantitative analysis method or detection method of ethylene oxide according to an embodiment of the present invention, the derivatization step in which a derivative reagent is added to the acid-decomposed sample to react is intended to improve the sensitivity to obtain lower detection limit and accurate results . In one embodiment, the derivatization is not limited as long as it can cause the derivatization reaction of 2-chloroethanol. The derivatization method is not limited, and may include, for example, silylation, acylation, and the like. As used herein, the term "derivative reagent" refers to a reagent capable of causing a derivative reaction of 2-chloroethanol. For example, derivatives reagent for silylation is N - tert - as, N, O- bis trimethylsilyl-trifluoromethyl-butyldimethylsilyl - N - - methyl trifluoromethyl Loa theta imide (tert -Butyldimethylsilyl- N -methyltrifluoroacetamide, MTBSFTA N ) But are not limited to, at least one of N, O-bis (trimethylsilyl) -trifluoro acetamide, BSTFA, and trimethyl chloro silane (TMCS). Also, for example, the acylated derivative reagent may include, but is not limited to, at least one of trifluoroacetic acid anhydride and heptafluorobutyric acid anhydride.

In the method for quantitative analysis or detection of ethylene oxide according to an embodiment of the present invention, the sample to be analyzed may be a food sample; An environmental sample comprising at least one of water and soil; And a biological sample containing one or more of blood or urine. In the present specification, the above-mentioned "food sample" is a concept covering all samples capable of being consumed. Specifically, the food sample may include both a natural state sample not subjected to cooking and a cooked state sample. As a more specific example, the food sample may be water, white fish.

In the method for quantitative analysis or detection of ethylene oxide according to an embodiment of the present invention, the step of decomposing the acid may further include a step of treating the sample to be analyzed with an acid and a salt, followed by heating and acid-decomposing the sample. As used herein, the terms "acid" and "salt" are intended to include both acids and salts capable of converting ethylene oxide to 2-chloroethanol. Specifically, the acid decomposing step may include a step of dissolving a water-soluble salt containing at least one acid and chlorine selected from the group consisting of hydrochloric acid, nitric acid and sulfuric acid, more specifically, sodium chloride (NaCl), potassium chloride (KCl) (NH ₄ Cl); and homogenizing the at least one salt; And heating the homogenized sample at a temperature of 50 ° C or more and less than 100 ° C for 10 to 50 minutes.

In addition, one embodiment of the present invention may further include concentrating the sample before the derivatization step to further improve the analytical sensitivity.

The present invention can provide a quantitative assay kit of ethylene oxide or a detection kit of ethylene oxide as one embodiment.

In one embodiment, the quantitative analysis kit or the detection kit comprises a reaction apparatus comprising an acid, a salt and a heating device for converting ethylene oxide into 2-chloroethanol; A derivative reagent of 2-chloroethanol; And a mass analyzer.

In one embodiment, the acid and the salt are not limited as long as it is an acid or a salt capable of converting ethylene oxide into 2-chloroethanol, and examples thereof include at least one acid selected from the group consisting of hydrochloric acid, nitric acid and sulfuric acid, More preferably at least one salt in the group consisting of sodium chloride (NaCl), potassium chloride (KCl) and ammonium chloride (NH ₄ Cl). In one embodiment, the heating device may include a boiler, but is not limited thereto, so long as it can heat the sample to a temperature of 50 ° C or more and less than 100 ° C. In one embodiment, the derivative reagent of 2-chloroethanol may be any reagent capable of causing a 2-chloroethanol derivative reaction, and may include, for example, a silylation reagent or an acylation reagent. In this case, the reagent for the silylated derivative is specifically N - tert - butyldimethylsilyl - N - methyl trifluoromethyl Loa theta imide (N - tert -Butyldimethylsilyl- N -methyltrifluoroacetamide, MTBSFTA), N, O- bis trimethylsilyl But are not limited to, at least one of N, O-bis- (trimethylsilyl) -trifluoroacetamide (BSTFA) and trimethylchlorosilane (TMCS). Also, for example, the acylated derivative reagent may include, but is not limited to, at least one of trifluoroacetic acid anhydride and heptafluorobutyric acid anhydride.

In one embodiment, the mass spectrometer comprises a concentration of derivatized 2-chloroethanol, ethylene oxide, 2-chloroethanol, or the like, such as silylated 2-chloroethanol, i.e., (2-chloroethoxy) , Concentration, and the like, as long as it can measure the concentration of the compound. The mass spectrometer may comprise, for example, gas chromatography mass spectrometry.

The present invention may be further embodied as an embodiment of a quantitative analysis kit for ethylene oxide, which may further include an instruction describing a quantitative analysis method of ethylene oxide according to one embodiment of the present invention described above.

In addition, the present invention may further comprise an indicator for describing the ethylene oxide detection method according to one embodiment of the present invention described above as a detection kit for ethylene oxide as one embodiment.

Hereinafter, the present invention will be described more specifically with reference to the following examples. However, the following examples are provided for illustrative purposes only in order to facilitate understanding of the present invention, and the scope and scope of the present invention are not limited thereto.

[Example 1]

Treatment of sample to be analyzed

The food samples were used as the target samples, and distilled water was used as the food samples.

Conical (Conical) to the internal standard solution after the food taken by the sample tube 10 g phenanthrene -d ₁₀ (phenanthrene-d ₁₀₎ solution (10 ㎍ / mL) was added to 50 ㎕, sodium chloride 2g, 1 M HCl 500μL The lid was then closed and homogenized sufficiently. The homogenized sample was placed in a constant-temperature water bath and heated at 80 ° C for 30 minutes to hydrolyze ethylene oxide into 2-coloethanol. The sample was taken out at room temperature.

MTBE (15 mL) was added to the sample at room temperature and extracted with a shaker for 20 minutes. After the extraction, the aqueous solution layer was discarded, and the organic solvent layer was separated, and then dehydrated with 1 g of anhydrous sodium sulfate and concentrated to 1 mL using a nitrogen concentrator.

To the concentrated sample was added N, O-bis (trimethylsilyl) -trifluoroacetamide (BSTFA) and trimethyl chloro silane (TMCS) in a ratio of 99: 1 v / v) solution (Sigma-Aldrich, Steinheim, Germany) was added and reacted at 60 ° C for 30 minutes to silylate (trimethylsilylate).

gas Chromatograph Mass spectrometer ( GC -MS) analysis

An Agilent 5975 C mass selective detector connected directly to a GC-MS instrument (Agilent Technologies, Inc., Santa Clara, Calif., USA, Agilent 6890 N gas chromatograph) was injected with 2 μl of the silylated sample.

The separation tube used was ultra-2 (cross-linked 5% phenylmethyl silicone, length 25 m, internal diameter 0.2 mm, film thickness 0.33 μm) and carrier gas was ultrapure (99.9999%) helium at a flow rate of 1 mL / Respectively. The temperature of the injection port was 250 ° C and a splitless injection mode was used. The oven conditions were set to warm from 50 to 300 < 0 > C. The electron energy used for ionization was 70 eV, and selected ion monitoring (SIM mode) was used. GC-MS operating conditions are shown in Table 1 below.

Condition Separator Ultra-2
(Cross-linked 5% phenylmethyl silicone, 25 m x 0.2 mm ID, 0.33 um film thickness) Carrier gas A flow rate of 1.0 mL / min of helium Injection mode Splitless mode Dose 2 μl Acquisition mode SIM mode in GC-MSD Ionization EI at 70 eV Solvent delay time 4 minutes Total time 28 minutes Temperature programming Initial 50 ° C # Heating rate (° C / min) Temperature (℃) Time (minutes) One 0 50 One 2 10 300 2

The standard solution of ethylene oxide was added to the distilled water in various concentrations and analyzed by GC-MS, which is shown in Fig. The calibration curves of the ethylene oxide in the food thus obtained are shown in Table 2 below.

Analyte Black curve Concentration range (/ / L) The regression line (y = ax + b) Linearity (r ² ) Ethylene oxide 1-500 y = 0.5169x + 0.0706 0.9983

As a result, a calibration curve with good linearity of 0.9983 was obtained at a concentration range of 5-500 ㎍ / L. The above results indicate that ethylene oxide contained in a sample can be detected and its concentration can be quantified by measuring and analyzing the concentration of ethylene oxide in a food sample according to the present invention.

On the other hand, the calibration curve can be obtained by the following method.

When analyzing ethylene oxide, analytical samples are quantitated using calibration curves prepared using internal standard method. As an internal reference material, phenanthrene-d ₁₀ is used. The detection limit is calculated by multiplying the standard deviation of the low concentration of 7 measurements by 3.14, and multiplying by 10 for the quantitation limit.

1) Creating a calibration curve

Standard calibration curves were prepared by adding a constant amount of internal standard (phenanthrene-d ₁₀ ) and standard ethylene oxide (ethylene oxide) to the representative medium, ranging from 5 to 500 ng / g . (2-chloroethoxy) trimethylsilane) was measured for the concentration of ethylene oxide by the concentration of ethylene oxide to determine the concentration ratio (standard substance concentration / internal standard substance concentration) of the x-axis and the instrument sensitivity ratio (Instrument sensitivity of (2-chloroethoxy) trimethylsilane / instrument sensitivity of internal standard material). In this case, the standard material is prepared by continuous dilution method and diluted with the last used solvent at the time of preparation in the working concentration range.

2) Concentration calculation

(2-chloroethoxy) trimethylsilane obtained when the sample is pretreated by instrumental analysis is multiplied by the concentration of the internal standard substance in the concentration ratio obtained by substituting the instrument sensitivity into the calibration curve, and the concentration is set as the sample concentration. However, when 2-chloroethanol is already contained in the sample itself, 2-chloroethanol contained in the original sample and 2-chloroethanol converted from ethylene oxide are simultaneously derivatized and detected. Therefore, the amount of ethylene oxide This may be overestimated. Therefore, one sample is analyzed including the conversion process, and one is analyzed excluding the conversion process. Only 2-chloroethanol contained in the original sample, which is not 2-chloroethanol converted from ethylene oxide, is derivatized and detected when the salt and the acid are added and the reaction is carried out to convert ethylene oxide to 2-chloroethanol during the pretreatment. do. When the difference between the concentration of the sample analyzed by converting ethylene oxide to 2-chloroethanol and the concentration of the sample not converting ethylene oxide into 2-chloroethanol was determined using ethylene oxide, the amount of ethylene oxide Can be measured accurately.

3) Detection limit

The method detection limit (MDL) is the minimum amount detectable at the 99% confidence level of the analytes present in a given medium and is reliably distinguished from zero, but quantified with appropriate precision Can not be the lowest concentration. Add the concentration expected to be the detection limit to the medium and measure it with the instrument after 7 repeated experiments in the same manner as the sample. The sensitivity of the instrument is substituted into the calibration curve and the standard deviation (σ) of the calculated concentrations is multiplied by 3.14 to be the detection limit.

4) Quantitative limit

The quantitation detection limit (QDL) is tested in the same manner as the method of calculating the detection limit. The sensitivity obtained by measuring the instrument is substituted into the calibration curve, and the standard deviation (σ) of the calculated concentrations is multiplied by 10 to be the quantitation limit.

[Experimental Example 1]

By comparing the method according to the present invention with the conventional analytical methods (Comparative Examples 1 and 2), the degree of accuracy of the ethylene oxide analysis of the method according to the present invention was confirmed. At this time, all of the above three methods were analyzed by converting ethylene oxide into 2-chloroethanol. Specifically, the method according to the present invention was carried out in the same manner as described in [Example 1] Headspace extraction method and Comparative Example 2 was carried out according to liquid-liquid extraction method. The experimental methods and the mass spectrometric conditions of Comparative Examples 1 and 2 are shown in FIGS. 4 and 5, and the results are shown in FIG.

As a result of the comparison between the method according to the present invention (Example 1) and the analytical results of Comparative Examples 1 and 2 which are conventional analytical methods, it can be confirmed that Example 1 has the lowest detection limit among the three methods. This means that in the process according to the present invention, the problem that ethylene oxide is not separated due to overlapping with acetaldehyde is converted into 2-chloroethanol and analyzed, so that it can be analyzed accurately without being disturbed by other substances.

While the present invention has been particularly shown and described with reference to specific embodiments thereof, those skilled in the art will readily appreciate that many modifications are possible in the exemplary embodiments without materially departing from the novel teachings and advantages of this invention. something to do. Accordingly, the actual scope of the present invention will be defined by the appended claims and their equivalents.

Claims (18)

An acid decomposition step in which the sample to be analyzed is heated under acidic conditions to convert ethylene oxide contained in the sample to 2-chloroethanol;
A derivatization step of reacting the acid-decomposed sample with a derivative reagent;
Measuring the concentration of the derivatized 2-chloroethanol in the derivatized sample; And
Analyzing the amount of ethylene oxide contained in the sample to be analyzed by calculating the amount of conversion of the ethylene oxide to 2-chloroethanol from the concentration of the derivatized 2-chloroethanol measured from the sample,
The step of analyzing the amount of ethylene oxide contained in the sample to be analyzed by calculating the amount of conversion of the ethylene oxide to 2-chloroethanol from the concentration of the derivatized 2-chloroethanol measured from the sample, A derivatization step of derivatizing the sample to be analyzed not subjected to the step; Measuring the concentration of the derivatized 2-chloroethanol in the derivatized sample; Wherein the concentration of the derivatized 2-chloroethanol measured from the sample in which the ethylene oxide is converted to 2-chloroethanol through the acid decomposing step and the concentration of the derivatized 2-chloroethanol measured from the analytical sample not subjected to the acid decomposition step And calculating an amount of conversion of ethylene oxide to 2-chloroethanol from the difference in the ethanol concentration. delete The method of quantitative analysis of ethylene oxide according to claim 1, wherein the derivatization is silylation or acylation. The method of claim 1, wherein the derivative reagent is N - tert - as, N, O- bis trimethylsilyl-trifluoromethyl-butyldimethylsilyl - N - - methyl trifluoromethyl Loa theta imide (tert -Butyldimethylsilyl- N -methyltrifluoroacetamide, MTBSFTA N ) A silylated derivative reagent comprising at least one of N, O-bis (trimethylsilyl) -trifluoro acetamide (BSTFA) and trimethyl chloro silane (TMCS); Or an acylating derivative reagent comprising at least one of Trifluoroacetic acid anhydride and Heptafluorobutyric acid anhydride. 2. The method of claim 1, wherein calculating the conversion of ethylene oxide to 2-chloroethanol comprises:
The conversion of the ethylene oxide to the 2-chloroethanol is carried out through the acid decomposition step, and the amount of conversion of the ethylene oxide to the 2-chloroethanol is calculated from the concentration of the derivatized 2-chloroethanol measured from the sample, Further comprising the step of quantifying 2-chloroethanol contained in the sample. The method according to claim 1, wherein the sample to be analyzed is a food sample; An environmental sample comprising at least one of water and soil; And a biological sample containing one or more of blood or urine. 2. The method of claim 1, wherein measuring the concentration of the derivatized 2-chloroethanol in the derivatized sample comprises measuring through a mass spectrometer. 2. The method according to claim 1,
Treating the sample to be analyzed with a water-soluble salt containing at least one acid selected from the group consisting of hydrochloric acid, nitric acid, and sulfuric acid and chlorine to homogenize the sample; And
And heating the homogenized sample at a temperature of 50 DEG C or more and less than 100 DEG C for 10 to 50 minutes. An acid decomposition step in which the sample to be analyzed is heated under acidic conditions to convert ethylene oxide contained in the sample to 2-chloroethanol;
A derivatization step of reacting the acid-decomposed sample with a derivative reagent;
Measuring the concentration of the derivatized 2-chloroethanol in the derivatized sample;
Calculating the amount of conversion of said ethylene oxide to 2-chloroethanol from the concentration of the derivatized 2-chloroethanol measured from said sample; And
And determining that the ethylene oxide in the sample to be analyzed is included if the conversion amount is greater than 0,
The step of calculating the amount of conversion of the ethylene oxide to 2-chloroethanol from the concentration of the derivatized 2-chloroethanol measured from the sample may include: a derivatization step of derivatizing a sample to be analyzed not subjected to the acid decomposition step; Measuring the concentration of the derivatized 2-chloroethanol in the derivatized sample; Wherein the concentration of the derivatized 2-chloroethanol measured from the sample in which the ethylene oxide is converted to 2-chloroethanol through the acid decomposing step and the concentration of the derivatized 2-chloroethanol measured from the analytical sample not subjected to the acid decomposition step Calculating the amount of ethylene oxide to be converted to 2-chloroethanol from the difference in the ethanol concentration. delete 10. The method of claim 9, wherein said derivatization is silylation or acylation. The method of claim 9 wherein the derivative reagent is N - tert - as, N, O- bis trimethylsilyl-trifluoromethyl-butyldimethylsilyl - N - - methyl trifluoromethyl Loa theta imide (tert -Butyldimethylsilyl- N -methyltrifluoroacetamide, MTBSFTA N ) A silylated derivative reagent comprising at least one of N, O-bis (trimethylsilyl) -trifluoro acetamide (BSTFA) and trimethyl chloro silane (TMCS); Or an acylated derivative reagent comprising at least one of trifluoroacetic acid anhydride and heptafluorobutyric acid anhydride. The method according to claim 9, wherein the sample to be analyzed is a food sample; An environmental sample comprising at least one of water and soil; And a biological sample containing one or more of blood or urine. 10. The method of claim 9, wherein measuring the concentration of the derivatized 2-chloroethanol in the derivatized sample comprises measuring through a mass spectrometer. A reaction apparatus comprising an acid, a salt and a heating apparatus for converting ethylene oxide into 2-chloroethanol;
A derivative reagent of 2-chloroethanol;
An indicator for describing the quantitative analysis method according to any one of claims 1 to 8; And
A mass spectrometry kit for quantitative analysis of ethylene oxide. delete A reaction apparatus comprising an acid, a salt and a heating apparatus for converting ethylene oxide into 2-chloroethanol;
A derivative reagent of 2-chloroethanol;
An indicator describing the quantitative assay method of any one of claims 9, 11 and 14; And
A mass spectrometer comprising an ethylene oxide detector kit. delete

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