CN110554133A - Detection method of prothioconazole residual quantity in rice - Google Patents
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Abstract
The invention discloses a method for detecting the residual amount of prothioconazole in rice, which comprises the following steps: pretreating a rice sample, weighing a proper amount of the rice sample, placing the rice sample in a triangular flask with a plug, adding glacial acetic acid acetonitrile mixed solution for oscillation extraction, filtering an extracting solution, salting out NaCl, violently oscillating, standing for layering, absorbing organic phase supernatant of half of the extracting solution, transferring the organic phase supernatant into a triangular flask with a ground opening, concentrating to be nearly dry, purifying the extracted concentrated solution by a Florisil silica chromatographic column, detecting by a high performance liquid chromatograph with an ultraviolet detector under a selected chromatographic condition, and quantifying by an external standard method. Under the conditions of sample preparation (extraction and purification) and detection provided by the invention, the prothioconazole and impurities in a rice matrix are well separated, the peak-appearing time is proper, and the methodological verification test research shows that the sensitivity, accuracy and precision of the established method all meet the technical requirements of pesticide residue determination, and the method is suitable for accurate and rapid analysis of the residual quantity of the prothioconazole in rice.
Description
Technical Field
The invention relates to pesticide residue detection, and in particular relates to a method for detecting the residue of prothioconazole in rice.
Background
Albendazole, the chemical name of which is 5- (propylthio) -1H-benzimidazol-2-yl methyl carbamate, and the chemical formula of which is C 12 H 15 N 3 O 2 S, Albendazole, a new compound developed in the United states 'SmithKline animal health laboratory' in 1972 and used for bacterial and parasitic infection of animals.
When the albendazole is applied to different crops for sterilization, part of pesticide residues inevitably exist along with the increase of the using amount of the albendazole, and the research on the albendazole analysis technology in different crops such as rice and the like is very necessary for ensuring the food safety and reducing the pesticide pollution. China has established that the temporary maximum residual limit (MRL value) of the albendazole in the brown rice is 0.1 mg/kg. At present, no published report is found on a residual analysis method of the albendazole in the plant matrix at home and abroad.
Disclosure of Invention
The invention aims to provide a method for analyzing residue of albendazole in rice, which is mainly used for measuring the content of albendazole residual in substrates such as rice, rice hulls, rice straws and the like, and has the characteristics of simplicity, accuracy, rapidness, reliability, low cost and easiness in mastering and popularization.
In order to achieve the purpose, the invention provides a method for detecting the residual quantity of albendazole in rice, which comprises the following steps:
Step one, sample pretreatment
The rice straw sample: cutting into small segments with length of 1 cm;
brown rice and rice hull samples: separating brown rice and rice hull with rice huller, pulverizing brown rice and rice hull with plant pulverizer respectively, sieving with 20 mesh sieve, and packaging in clean sealed plastic bag;
Step two, accurately weighing the sample of the brown rice, the rice hulls or the rice straws pretreated in the step one, placing the sample in a container, adding glacial acetic acid acetonitrile with the mass concentration of 1% to submerge the sample of the brown rice, the rice hulls or the rice straws, oscillating and extracting the sample at the temperature of 30-35 ℃ for 30-60 min, filtering the sample by a small funnel, salting out the filtrate by NaCl, standing and layering the filtrate after violent oscillation, absorbing half of organic phase supernatant of the extracting solution, transferring the organic phase supernatant into a 250mL ground triangular flask, and concentrating the organic phase supernatant at the temperature of 45 ℃ on a rotary evaporator until the organic phase supernatant is nearly dry to obtain an extracting concentrated solution;
Purifying the prepared extraction concentrated solution by a Florisil chromatographic column, wherein the Florisil chromatographic column is sequentially filled with absorbent cotton, anhydrous sodium sulfate with the thickness of 2cm, 5g of Florisil and anhydrous sodium sulfate with the thickness of 2cm from bottom to top; after the Florisil chromatographic column is filled, pre-leaching with 15mL of methanol, and discarding pre-leaching solution; then transferring all the extracted concentrated solution into a Florisil chromatographic column, leaching with 10mL of methanol, collecting all leacheate, transferring into a 250mL triangular flask with a plug, concentrating on a rotary evaporator at 45 ℃ until the leacheate is nearly dry, metering the volume to 5.0mL with chromatographic methanol, and filtering with a 0.45-micron microporous filter membrane to form a sample solution to be detected;
Selecting HPLC chromatographic conditions that the high performance liquid chromatograph is a high performance liquid chromatograph with an ultraviolet detector, the length of a chromatographic column is 250mm multiplied by 4.6mm, the particle size of a ZORBAX Eclipse XDB-C 18 chromatographic column is 5u, the column temperature is 35 ℃, the flow rate is 0.6mL/min, the sample introduction amount is 20uL, the mobile phase is a mixed solution consisting of methanol and an aqueous solution, the volume ratio of the methanol to the aqueous solution is 72: 28, and the wavelength is 245 nm;
Step five, accurately weighing the standard product of the albendazole, dissolving the standard product of the albendazole with chromatographic methanol to prepare a standard mother solution, then respectively preparing the standard mother solution of the albendazole into a standard working solution of the albendazole by adopting a gradient dilution method, respectively preparing the standard working solution of the albendazole with the albendazole mass concentration of 0.05, 0.10, 0.50, 1.00 and 5.00mg/L, respectively injecting the standard working solution into a high performance liquid chromatograph, simultaneously satisfying the HPLC chromatographic conditions of the step four for determination, respectively drawing a standard working curve of the albendazole by taking the albendazole mass concentration x as a horizontal coordinate and taking the corresponding chromatographic peak area y as a vertical coordinate, and further obtaining a standard curve equation y of the albendazole, wherein the standard curve equation y is 94.713x +0.4029, and the correlation coefficient R 2 is 1;
And step six, injecting the sample solution to be detected prepared in step three into the high performance liquid chromatograph selected in step four, detecting according to the chromatographic conditions in step four, and substituting the measured chromatographic peak area into the standard curve equation in step five to obtain the mass concentration of the prothioconazole in the sample.
compared with the prior art, the invention has the beneficial effects that:
The invention researches and establishes a high performance liquid chromatograph detection and analysis method for the residue of the albendazole in the chaff, the rice and the rice straws, and provides scientific basis for the dietary risk assessment of the albendazole and the residue monitoring of the albendazole in agricultural products.
The method uses a peak area external standard method for quantification, so that the standard curve has good linearity and good reproducibility, high-efficiency separation is achieved, and the residual quantity of the albendazole in the rice is effectively detected.
The standard working solution of the albendazole is added into the rice blank sample, so that the mass concentrations of the albendazole in the brown rice are respectively 0.05, 0.10, 1.00 and 5.00mg/kg, and the mass concentrations of the albendazole in the rice husks and the rice straws are respectively 0.05, 0.10 and 1.00 mg/kg; repeating each concentration for 5 times, and performing sample preparation and analysis determination by the established method, wherein the average addition recovery rate of the albendazole in the brown rice is 84-115%, and the relative standard deviation is 2-4%; the average adding recovery rate of the albendazole in the chaff is 76-102%, and the relative standard deviation is 3-7%; the average adding recovery rate of the albendazole in the rice straws is 78-99%, and the relative standard deviation is 3-8%; the sensitivity, accuracy and precision of the method all meet the requirement of pesticide residue detection, and the method is suitable for accurate and rapid analysis of the residue of the prothioconazole in the rice.
The method can effectively extract the albendazole from the rice and effectively purify the influence of other impurities in the rice on subsequent detection, thereby improving the detection accuracy.
Drawings
Fig. 1 is a standard graph of example 1, wherein the standard curve equation is y 94.713x +0.4029, R 2 is 1;
FIG. 2 is a chromatogram of a standard solution (1mg/L) of prothioconazole from example 1.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to the specific embodiments, but the present invention is not limited thereto.
Example 1:
(1) sample pretreatment
the rice straw sample: the collected rice straw sample is cut into about 1 cm. Brown rice and rice hull samples: separating the husks and the brown rice by using a rice huller, crushing the husks and the brown rice by using a plant crusher respectively, sieving the crushed husks and the brown rice by using a 20-mesh sieve, and filling the crushed husks and the brown rice in a clean sealed plastic bag.
(2) Preparation of sample solution to be tested
Extraction of alphos
Accurately weighing 10.0g of a pretreated sample (brown rice, chaff or straw), placing the sample into a 250mL triangular flask with a plug, adding 40mL of acetonitrile and 0.4 mL of glacial acetic acid (60 mL of acetonitrile and 0.6mL of glacial acetic acid of chaff or straw), oscillating and extracting at 25 ℃ for 1h, filtering through a small funnel, salting out the filtrate by 2g of NaCl, standing and layering after violent oscillation, sucking 20mL of organic phase supernatant (30 mL of organic phase supernatant is taken from chaff or straw), transferring into a 250mL triangular flask with a ground opening, concentrating to be nearly dry on a rotary evaporator (45 ℃), and purifying by using a Florisil silica chromatographic column.
b purification of the extract
purifying the extracted concentrated solution of the sample by a Florisil chromatographic column, wherein the Florisil chromatographic column is sequentially filled with a little absorbent cotton, anhydrous sodium sulfate with the thickness of 2cm, 5g of Florisil and anhydrous sodium sulfate with the thickness of 2cm from bottom to top; after the Florisil chromatographic column is filled, pre-leaching with 15mL of methanol, and discarding pre-leaching solution; and transferring all the extract concentrated solution into a Florisil chromatographic column, eluting with 10mL of methanol, collecting all eluates, transferring into a 250mL triangular flask with a plug, concentrating on a rotary evaporator (45 ℃) until the eluates are nearly dry, metering the volume to 5.0mL by using chromatographic methanol, and filtering with a 0.45-micron microporous filter membrane for HPLC detection.
(3) Preparation of Standard solutions
Accurately weighing 0.1010g (accurate to 0.0001g) of a standard prothioconazole (with the purity of 99.9 percent), transferring the standard prothioconazole into a 100mL brown volumetric flask, dissolving the standard prothioconazole with chromatographic methanol, and preparing a standard mother solution with the mass concentration of the prothioconazole of 1000.00 mg/L; then, the standard mother liquor of the albendazole is respectively taken by adopting a gradient dilution method to prepare standard working solution, so that the mass concentration of the albendazole is 0.05, 0.10, 0.50, 1 and 5.00 mg/L.
(4) High performance liquid chromatography
The chromatographic conditions for the selected HPLC assay were HPLC, i.e., a 1260-type HPLC (Agilent, USA) UV detector, a ZORBAX Eclipse XDB-C 18 column (4.6 mm. times.250 mm, 5 μm), a column temperature of 35 deg.C, a flow rate of 0.6mL/min, a sample size of 20uL, a mobile phase of methanol in aqueous solution (72: 28, v/v), and a wavelength of 245nm, and the relative retention time of the standard substance prothioconazole was about 13min under the above chromatographic conditions (see FIG. 2).
(5) Drawing of standard curve
The standard solutions prepared in step (3) are all injected into a high performance liquid chromatograph, and are measured under the HPLC detection conditions selected in step (4), a standard working curve of the albendazole is drawn by taking the mass concentration (x, mg/L) of the albendazole as an abscissa and the corresponding peak area (y) as an ordinate, the standard curve equation y of the albendazole is obtained as 94.713x +0.4029(R 2 is 1), and the peak area of the albendazole is obtained as shown in table 1, and the standard curve diagram is shown in fig. 1.
TABLE 1 Standard Curve for Prothioconazole
As can be seen from Table 1, the peak area of prothioconazole in a certain linear range has a very good linear relationship with the mass concentration, and the correlation coefficient is equal to 1.
(6) method verification
Respectively adding standard working solutions of the albendazole into blank control samples of the brown rice, the chaff and the rice straw to ensure that the mass concentration of the albendazole in the brown rice is 0.05, 0.10, 1.00 and 5.00mg/kg respectively, and the mass concentration of the albendazole in the chaff and the rice straw is 0.05, 0.10 and 1.00mg/kg respectively; each concentration was repeated 5 times, measured by the above selected analysis and detection method, and the recovery rate was calculated. The results are shown in Table 2.
table 2 recovery of prothioconazole from rice straw, brown rice and chaff and its relative standard deviation (n ═ 5)
under the selected HPLC detection condition, the limit of detection of the albendazole is 0.05mg/kg, and the limit of quantification of the albendazole in the brown rice, the chaff and the straw is 0.05 mg/kg; the lowest detection limit indicates that the method can detect substances with lower content. Therefore, the method can be used for accurately analyzing the sample and has higher sensitivity.
The invention establishes the HPLC method for detecting the albendazole in the rice, the standard curve equation is y-94.682 x +0.5244, the correlation coefficient R 2 is 1, the correlation is better, the average adding recovery rate of the albendazole in the brown rice is 84-115%, the relative standard deviation is 2-4%, the average adding recovery rate of the albendazole in the chaff is 76-102%, the relative standard deviation is 3-7%, the average adding recovery rate of the albendazole in the rice straw is 78-99%, and the relative standard deviation is 3-8%, and the sensitivity, the accuracy and the precision of the method all meet the requirements of pesticide residue detection.
(7) Calculation of measurement result of residual amount of sample solution
And (3) carrying out HPLC (high performance liquid chromatography) measurement on the sample solution under the selected chromatographic detection condition, measuring the chromatographic peak area of the albendazole in the sample solution, and substituting the chromatographic peak area into the following formula to obtain the residual amount (mass concentration) of the albendazole in the sample solution.
The calculation formula for prothioconazole in the sample is as follows:
Wherein: x- - -the residual amount of prothioconazole in the sample, mg/kg; c, calculating the sample injection concentration according to the peak area of the sample through a standard curve: mg/L; m represents the sample weight and g represents the total weight of the sample; v- - -constant volume, mL.
(8) Determination of actual samples
the 10% albendazole suspending agent is applied to east-coast countries of hibiscus areas collected from Changsha city, Hunan province in 2018, the suspending agent is applied by mixing water and spraying in the growth period of rice according to the effective component dosage of 150a.i.g/ha (the dosage of the preparation is 100 g/mu), and the water mixing amount per mu is as follows: 50L, applying the pesticide for 3 times, wherein the application interval period is 7d, and preventing and treating the bacterial leaf streak of the rice; respectively collecting rice and chaff samples 2h, 7d, 14d, 21d and 28d after the last pesticide application, respectively collecting rice straw samples 14d and 21d after the last pesticide application, and detecting the residual quantity of the albendazole. Some results are shown in tables 3-5.
TABLE 3 residual amount of prothioconazole in brown rice
TABLE 4 residual amount of prothioconazole in chaff
TABLE 5 residual amount of prothioconazole in rice straw
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not intended to limit the present invention in any way, and the skilled in the art should cover within the scope of the present invention the modifications and equivalents of the embodiments within the technical scope of the present invention.
Claims (1)
1. A method for detecting the residual amount of prothioconazole in rice is characterized by comprising the following steps:
Step one, sample pretreatment
The rice straw sample: cutting into small segments with the length of about 1 cm;
brown rice and rice hull samples: separating brown rice and rice hull with rice huller, pulverizing brown rice and rice hull with plant pulverizer respectively, sieving with 20 mesh sieve, and packaging in clean sealed plastic bag;
Step two, accurately weighing the sample of the brown rice, the rice hulls or the rice straws pretreated in the step one, placing the sample in a container, adding glacial acetic acid acetonitrile with the mass concentration of 1% to submerge the sample of the brown rice, the rice hulls or the rice straws, oscillating and extracting the sample at the temperature of 30-35 ℃ for 30-60 min, filtering the sample by a small funnel, salting out the filtrate by NaCl, standing and layering the filtrate after violent oscillation, absorbing half of organic phase supernatant of the extracting solution, transferring the organic phase supernatant into a 250mL ground triangular flask, and concentrating the organic phase supernatant at the temperature of 45 ℃ on a rotary evaporator until the organic phase supernatant is nearly dry to obtain an extracting concentrated solution;
Purifying the prepared extraction concentrated solution by a Florisil chromatographic column, wherein the Florisil chromatographic column is sequentially filled with absorbent cotton, anhydrous sodium sulfate with the thickness of 2cm, 5g of Florisil and anhydrous sodium sulfate with the thickness of 2cm from bottom to top; after the Florisil chromatographic column is filled, pre-leaching with 15mL of methanol, and discarding pre-leaching solution; then transferring all the extracted concentrated solution into a Florisil chromatographic column, leaching with 10mL of methanol, collecting all leacheate, transferring into a 250mL triangular flask with a plug, concentrating on a rotary evaporator at 45 ℃ until the leacheate is nearly dry, metering the volume to 5.0mL with chromatographic methanol, and filtering with a 0.45-micron microporous filter membrane to form a sample solution to be detected;
Selecting HPLC chromatographic conditions that the high performance liquid chromatograph is a high performance liquid chromatograph with an ultraviolet detector, the length of a chromatographic column is 250mm multiplied by 4.6mm, the particle size of a ZORBAX Eclipse XDB-C 18 chromatographic column is 5u, the column temperature is 35 ℃, the flow rate is 0.6mL/min, the sample introduction amount is 20uL, the mobile phase is a mixed solution consisting of methanol and an aqueous solution, the volume ratio of the methanol to the aqueous solution is 72: 28, and the wavelength is 245 nm;
Step five, accurately weighing the standard product of the albendazole, dissolving the standard product of the albendazole with chromatographic methanol to prepare a standard mother solution, then respectively preparing the standard mother solution of the albendazole into a standard working solution of the albendazole by adopting a gradient dilution method, respectively preparing the standard working solution of the albendazole with the albendazole mass concentration of 0.05, 0.10, 0.50, 1.00 and 5.00mg/L, respectively injecting the standard working solution into a high performance liquid chromatograph, simultaneously satisfying the HPLC chromatographic conditions of the step four for determination, respectively drawing a standard working curve of the albendazole by taking the albendazole mass concentration x as a horizontal coordinate and taking the corresponding chromatographic peak area y as a vertical coordinate, and further obtaining a standard curve equation y of the albendazole, wherein the standard curve equation y is 94.713x +0.4029, and the correlation coefficient R 2 is 1;
and step six, injecting the sample solution to be detected prepared in step three into the high performance liquid chromatograph selected in step four, detecting according to the chromatographic conditions in step four, and substituting the measured chromatographic peak area into the standard curve equation in step five to obtain the mass concentration of the prothioconazole in the sample.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108828110A (en) * | 2018-09-11 | 2018-11-16 | 广东出入境检验检疫局检验检疫技术中心 | The measuring method of benzimidazoles residues residual quantity in one breeder fat |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108896694A (en) * | 2018-07-05 | 2018-11-27 | 中国农业科学院农业质量标准与检测技术研究所 | A kind of remaining LC-QToF-MS Screening analysis method of pesticide in animal food |
| CN108828110A (en) * | 2018-09-11 | 2018-11-16 | 广东出入境检验检疫局检验检疫技术中心 | The measuring method of benzimidazoles residues residual quantity in one breeder fat |
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Application publication date: 20191210 |
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