CN102200531A - Method for detecting cartap residue in cereal grain with gas chromatography - Google Patents
Method for detecting cartap residue in cereal grain with gas chromatography Download PDFInfo
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- CN102200531A CN102200531A CN2011100762571A CN201110076257A CN102200531A CN 102200531 A CN102200531 A CN 102200531A CN 2011100762571 A CN2011100762571 A CN 2011100762571A CN 201110076257 A CN201110076257 A CN 201110076257A CN 102200531 A CN102200531 A CN 102200531A
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Abstract
The invention relates to a method for detecting a method for detecting cartap residue in cereal grain with gas chromatography. The method comprises the following steps of: adding a diluted hydrochloric acid solution in a sample to be detected; fully processing with ultrasound and then centrifuging; purifying supernate with normal hexane and activated carbon; regulating pH value, then extracting with normal hexane; filtering extracting liquid with a membrane for gas chromatography; removing cartap standard liquid; diluting into a series of standard solutions with different concentrations by using carbinol; analyzing after extracting; and fixing quantity with an external standard method. For the cartap residue in the cereal grain, the method has detection limit up to 0.05mg/kg, average recovery rate of being between 75.5% and 106.1% and relative standard deviation of being 4.1% and 8.7%. The method for detecting the cartap residue in the cereal grain is simple, convenient, quick and sensitive and the recovery rate and detection limit of the method both can reach daily detection requirements. Therefore, the invention provides a reliable and feasible method for detecting the cartap residue in the cereal grain, thereby being capable of meeting research and production requirements.
Description
Technical field
The present invention relates to the assay method of cartap residual quantity in the Cereals, particularly relate to the assay method of a kind of vapor-phase chromatography cartap residual quantity in the Cereals.
Background technology
Cartap (cartap), Chinese commodity are called Padan, and chemistry is called 1,3-two (carbamyl sulphur)-2-dimethylaminopropanecompounds.Cartap is a sandworm toxin insecticide, multiple effect such as inhale stomach toxicity in having, tag, and effect is rapid, and the lasting period is longer, and insecticidal spectrum is wide, has the long longevity of residure, uses more extensive.Cartap is used for the Cereals class and is mainly used in control rice borer, rice plant skipper, leaf-roller, planthopper, rice leafhopper etc.GB2763-2005 is 0.1mg/kg to the maximum residue limit of cartap in the rice, and the detection method of quoting is GB/T 5009.145-2003.This method complicated operation, the recovery is low.Therefore set up a kind of quick, accurate, convenient and economic detection method, help monitoring the residual quantity of cartap in the Cereals, thereby ensure edible safety.
Summary of the invention
Technical matters to be solved by this invention is, overcome the interference of pre-treatment mesostroma, by groping the extract optium concentration, best extraction time, best extraction pH value and optimum chromatogram condition and the assay method of a kind of vapor-phase chromatography to cartap residual quantity in the Cereals is provided.
For achieving the above object, the present invention takes following design proposal:
A kind of vapor-phase chromatography of the present invention comprises the steps: the assay method of cartap residual quantity in the Cereals
Accurately take by weighing 2.0000g (be accurate to ± 0.0001g) evenly sample adds 20mL 0.05mol/L aqueous hydrochloric acid solution in 50mL tool plug centrifuge tube, ultrasonic Extraction 20min at the centrifugal 5min of 5000r/min, obtains supernatant then.
Supernatant is changed in another 50mL tool plug centrifuge tube, add 20mL normal hexane and 0.1g activated charcoal, vortex extracts 1min, in the centrifugal 5min of 5000r/min, inhales and abandons upper organic phase; Add the 20mL normal hexane again, repeat once.
Solution after the extraction is filled in another tool plug centrifuge tube, regulates the pH value to 8.5-9.0 with the Na0H aqueous solution of 2mol/L then, add the NaHCO of 5mL 50g/L
3Aqueous solution adds the 4.00mL normal hexane again, and vortex extracts 1min, in the centrifugal 5min of 5000r/min, upper organic phase is crossed film, air feed phase chromatographic determination.
Pipette cartap standard items, use liquid, air feed analysis of hplc after extracting for standard with concentration gradient with the methyl alcohol dilution with the methyl alcohol preparation.
Utilization is equipped with the gas chromatograph of electron capture detector that titer and sample treatment solution are detected;
The computing formula of cartap is in the sample:
X＝(C×V×1000)/(m×1000)
In the formula: (this formula form is consistent with other patented claim)
The content of cartap in the X-sample, unit are every kilogram (mg/kg) of milligram;
C-is through looking into the concentration that typical curve calculates gained sample introduction liquid, and unit is (μ g/mL);
V-sample constant volume, unit are milliliter (mL);
The m-sample weighting amount, unit is gram (g);
Preferably, described extraction solvent is a 0.05mol/L hydrochloric acid, and cartap is converted into the form of hydrochloride, and the part of forgoing is simultaneously disturbed.
Preferably, the ultrasonic Extraction time is 20min, guarantees to extract fully.
Preferably, the NaOH aqueous solution is regulated the pH value to 8.5-9.0, adds the NaHCO of 5mL 50g/L
3Aqueous solution adds the 4mL n-hexane extraction again, guarantees that the cartap hydrochloride is converted into the molecular state cartap, is beneficial to organic solvent extraction.
Preferably, described sample to be tested adopts mass concentration to operate and calculate in whole preparation process.
The described gas chromatograph that utilizes to the condition that sample treatment solution detects is:
Chromatographic column: DB-1701,30m * 0.25mm (internal diameter), 0.25 μ m (thickness);
Injection port: 250 ℃;
Input mode: do not shunt;
Sampling volume: 1.0 μ L;
Column temperature: 70 ℃ (keeping 1min), being warming up to 200 ℃ (keeping 10min) with 10 ℃/min, 30 ℃/min is warming up to 270 ℃ (keeping 5min);
Flow velocity: 1.00mL/min (constant linear velocity);
Detecting device: electron capture detector;
Detector temperature: 280 ℃.
And qualitative according to retention time, the external standard peak area method is quantitative.
Advantage of the present invention is: adopt the assay method of a kind of vapor-phase chromatography of the present invention to cartap residual quantity in the Cereals, effectively, RSD detects and is limited to 0.05mg/kg less than 10% fast.This shows that method of the present invention be to detect the residual quantity of cartap in the Cereals, a kind of method of implementing be convenient to reliably be provided, can satisfy research and produce in needs.
Embodiment
Embodiment 1, and the precision of cartap residual quantity and the recovery detect in the Cereals:
Accurately take by weighing 2.0005g (be accurate to ± even rice after 0.0001g) pulverizing adds 20mL 0.05mol/L hydrochloric acid solution in 50mL tool plug centrifuge tube, ultrasonic Extraction 20min, centrifugal 5min under the 5000r/min rotating speed obtains supernatant then.
Supernatant is changed in another 50mL tool plug centrifuge tube, add 20mL normal hexane and 0.1g activated charcoal, vortex extracts 1min, and is centrifugal, inhales and abandons upper organic phase; Add the 20mL normal hexane again, repeat once.
Solution after the extraction is filled in another tool plug centrifuge tube, regulates pH value to 8.5～9.0 with the NaOH aqueous solution of 2mol/L then, add the NaHCO of 5mL 50g/L
3Aqueous solution adds the 4.00mL normal hexane again, and vortex extracts 1min, in the centrifugal 5min of 5000r/min, upper organic phase is crossed film, air feed phase chromatographic determination.
Get cartap standard items (national standard material center) the 100 μ g/mL of methyl alcohol preparation, 10 times of dilute with waters use liquid as standard, dilution is the standard use liquid of 0.1,0.2,0.5,1.0 μ g/mL again, getting each standard of 4.00mL uses liquid in 50mL tool plug centrifuge tube, regulate pH value to 8.5～9.0 with the NaOH aqueous solution of 2mol/L then, add the NaHCO of 5mL 50g/L
3Aqueous solution adds the 4.00mL normal hexane again, and vortex extracts 1min, in the centrifugal 5min of 5000r/min, upper organic phase is crossed film, air feed phase chromatographic determination.
Detecting instrument is existing Agilent 7890A gas chromatograph:
Testing conditions is:
Chromatographic column: DB-1701,30m * 0.25mm (internal diameter), 0.25 μ m (thickness);
Injection port: 250 ℃;
Input mode: do not shunt;
Sampling volume: 1.0 μ L;
Column temperature: 70 ℃ (keeping 1min), being warming up to 200 ℃ (keeping 10min) with 10 ℃/min, 30 ℃/min is warming up to 270 ℃ (keeping 5min);
Flow velocity: 1.00mL/min (constant linear velocity);
Detecting device: electron capture detector;
Detector temperature: 280 ℃.
Qualitative according to retention time, the external standard peak area method is quantitative.
The computing formula of cartap is in the sample:
X＝(C×V×1000)/(m×1000) (1)
In the formula:
The content of cartap in the X-sample, unit are every kilogram (mg/kg) of milligram;
C-is through looking into the concentration that typical curve calculates gained sample introduction liquid, and unit is (μ g/mL);
V-sample constant volume, unit are milliliter (mL);
The m-sample weighting amount, unit is gram (g);
In the sample residual quantity of cartap by formula (1) calculate, the result is as follows:
Embodiment 2, the detection of the cartap residual quantity precision and the recovery in the Cereals:
Accurately take by weighing 2.0105g (be accurate to ± even wheat after 0.0001g) pulverizing adds 20mL 0.05mol/L hydrochloric acid solution in 50mL tool plug centrifuge tube, ultrasonic Extraction 20min at the centrifugal 5min of 5000r/min, obtains supernatant then.
Supernatant is changed in another 50mL tool plug centrifuge tube, add 20mL normal hexane and 0.1g activated charcoal, vortex extracts 1min, in the centrifugal 5min of 5000r/min, inhales and abandons upper organic phase; Add the 20mL normal hexane again, repeat once.
Solution after the extraction is filled in another tool plug centrifuge tube, regulates pH value to 8.5～9.0 with the NaOH aqueous solution of 2mol/L then, add the NaHCO of 5mL 50g/L
3Aqueous solution adds the 4mL normal hexane again, and vortex extracts 1min,, upper organic phase is transferred in the sample introduction bottle air feed phase chromatographic determination in the centrifugal 5min of 5000r/min with suction pipe.
Get cartap standard items (national standard material center) the 100 μ g/mL of methyl alcohol preparation, 10 times of dilute with waters use liquid as standard, dilution is the standard use liquid of 0.1,0.2,0.5,1.0 μ g/mL again, getting each standard of 4.00mL uses liquid in 50mL tool plug centrifuge tube, regulate pH value to 8.5～9.0 with the NaOH aqueous solution of 2mol/L then, add the NaHCO of 5mL 50g/L
3Aqueous solution adds the 4.00mL normal hexane again, and vortex extracts 1min,, upper organic phase is transferred in the sample introduction bottle air feed phase chromatographic determination in the centrifugal 5min of 5000r/min with suction pipe.
Detecting instrument is existing Agilent 7890A gas chromatograph:
Testing conditions is:
Chromatographic column: DB-1701,30m * 0.25mm (internal diameter), 0.25 μ m (thickness);
Injection port: 250 ℃;
Input mode: split ratio not;
Sampling volume: 1.0 μ L;
Column temperature: 70 ℃ (keeping 1min), being warming up to 200 ℃ (keeping 10min) with 10 ℃/min, 30 ℃/min is warming up to 270 ℃ (keeping 5min);
Flow velocity: 1.00mL/min (constant linear velocity);
Detecting device: electron capture detector;
Detector temperature: 280 ℃.
Qualitative according to retention time, the external standard peak area method is quantitative.
In the sample residual quantity of cartap by formula (1) calculate, the result is as follows:
Obviously, those of ordinary skill in the art can measure the cartap residual quantity in the Cereals by gas chromatograph with a kind of of invention.
The foregoing description is only for the usefulness that the present invention is described; and be not to be limitation of the present invention; the those of ordinary skill in relevant technologies field; without departing from the present invention; can also make various variations and modification; therefore all technical schemes that are equal to also should belong to category of the present invention, and scope of patent protection of the present invention should be limited by each claim.
Claims (7)
1. a vapor-phase chromatography is to the assay method of cartap residual quantity in the Cereals, and it is characterized in that: described assay method comprises the steps:
Accurately take by weighing 2.0000g (be accurate to ± 0.0001g) evenly sample adds 20mL 0.05mol/L hydrochloric acid solution in 50mL tool plug centrifuge tube, ultrasonic Extraction 20min at the centrifugal 5min of 5000r/min, obtains supernatant then.
Supernatant is changed in another 50mL tool plug centrifuge tube, add 20mL normal hexane and 0.1g activated charcoal, vortex extracts 1min, in the centrifugal 5min of 5000r/min, inhales and abandons upper organic phase; Add the 20mL normal hexane again, repeat once.
Solution after the extraction is filled in another tool plug centrifuge tube, regulates the pH value to 8.5-9.0 with the Na0H aqueous solution of 2mol/L then, add the NaHCO of 5mL 50g/L
3Aqueous solution adds the 4.00mL normal hexane again, and vortex extracts 1min, in the centrifugal 5min of 5000r/min, upper organic phase is transferred in the sample introduction bottle with suction pipe, for the gas Chromatographic Determination that is equipped with electron capture detector.
Pipette cartap standard items, use liquid, air feed analysis of hplc after extracting for standard with concentration gradient with the methyl alcohol dilution with the methyl alcohol preparation.
Utilize gas chromatograph that standard solution and sample treatment solution are detected;
The computing formula of cartap is in the sample:
X＝(C×V×1000)/(m×1000)
In the formula: (formula needs to revise)
The content of cartap in the X-sample, unit are every kilogram (mg/kg) of milligram;
C-is through looking into the concentration that typical curve calculates gained sample introduction liquid, and unit is (μ g/mL);
V-sample constant volume, unit are milliliter (mL);
The m-sample weighting amount, unit is gram (g);
Result of calculation remains to 2 significant digits.
2. a kind of vapor-phase chromatography according to claim 1 is to the assay method of cartap residual quantity in the Cereals, it is characterized in that: described 0.05mol/L aqueous hydrochloric acid solution extracts, cartap is stable under acid condition, ionic condition with hydrochloride exists, better controlled the interference of impurity, and guaranteed the recovery.
3. a kind of vapor-phase chromatography according to claim 1 is characterized in that the assay method of cartap residual quantity in the Cereals: ultrasonic Extraction 20min then at the centrifugal 5min of 5000r/min, obtains having best mixing extraction efficiency under this condition of supernatant.
4. a kind of vapor-phase chromatography according to claim 1 is to the assay method of cartap residual quantity in the Cereals, it is characterized in that: add 20mL normal hexane and 0.1g activated charcoal, vortex extracts 1min, in the centrifugal 5min of 5000r/min, upper organic phase is abandoned in suction, can remove grease and pigment impurity in the sample under this condition, guarantee the recovery.
5. a kind of vapor-phase chromatography according to claim 1 is characterized in that the assay method of cartap residual quantity in the Cereals: the NaOH aqueous solution of 2mol/L is regulated the pH value to 8.5-9.0, adds the NaHCO of 5mL 50g/L
3Aqueous solution, with solution furnishing alkali condition, the cartap hydrochloride changes into molecular state, is extracted by hexane solution easily.
6. a kind of vapor-phase chromatography according to claim 1 is characterized in that the assay method of cartap residual quantity in the Cereals: the described gas chromatograph that utilizes to the condition that sample treatment solution detects is:
Chromatographic column: DB-1701,30m * 0.25mm, 0.25 μ m
Injection port: 250 ℃
Input mode: do not shunt
Sampling volume: 1.0 μ L
Column temperature: 70 ℃ (keeping 1min), being warming up to 200 ℃ (keeping 10min) with 10 ℃/min, 30 ℃/min is warming up to 270 ℃ (keeping 5min)
Flow velocity: 1.00mL/min
Detecting device: electron capture detector
Detector temperature: 280 ℃.
Has good separating effect under this condition.
7. a kind of vapor-phase chromatography according to claim 1 is characterized in that the assay method of cartap residual quantity in the Cereals: the instrument utilization comparatively gas chromatograph of general, suitable outfit electron capture detector detects cartap residual quantity in the Cereals.
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| CN2011100762571A CN102200531A (en) | 2011-03-29 | 2011-03-29 | Method for detecting cartap residue in cereal grain with gas chromatography |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110632215A (en) * | 2019-10-31 | 2019-12-31 | 中验检测股份有限公司 | Method for detecting cartap in tea |
| CN110824089A (en) * | 2019-11-27 | 2020-02-21 | 日照健安检测技术服务有限公司 | Method for rapidly detecting cartap residue in vegetables |
-
2011
- 2011-03-29 CN CN2011100762571A patent/CN102200531A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 吴刚 等: "气相色谱-微池电子捕获检测器分析茶叶中杀螟丹的残留", 《色谱》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110632215A (en) * | 2019-10-31 | 2019-12-31 | 中验检测股份有限公司 | Method for detecting cartap in tea |
| CN110824089A (en) * | 2019-11-27 | 2020-02-21 | 日照健安检测技术服务有限公司 | Method for rapidly detecting cartap residue in vegetables |
| CN110824089B (en) * | 2019-11-27 | 2022-04-12 | 日照健安检测技术服务有限公司 | Method for rapidly detecting cartap residue in vegetables |
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Application publication date: 20110928 |