CN108287201B - Method for detecting cyantraniliprole and metabolite J9Z38 in pork - Google Patents
Method for detecting cyantraniliprole and metabolite J9Z38 in pork Download PDFInfo
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Abstract
The invention provides a method for detecting cyantraniliprole and metabolite J9Z38 in pork, which comprises the following steps: extracting, purifying, measuring, and performing an addition recovery test to obtain the addition recovery and Relative Standard Deviation (RSDs) of cyantraniliprole and J9Z 38; detecting the minimum detection amount of cyantraniliprole and J9Z 38; the lowest detection concentration of cyantraniliprole and J9Z38 in pork is obtained. The invention establishes an analysis and detection method of cyantraniliprole in pork and a metabolite J9Z38 thereof; the method has the advantages of simple pretreatment process, high recovery rate, good repeatability, good purification and separation effects, low minimum detection concentration and suitability for analysis and detection of cyantraniliprole and metabolite J9Z38 in pork.
Description
Technical Field
The invention relates to pesticide detection, in particular to a method for detecting cyantraniliprole and a metabolite J9Z38 in pork.
Background
Cyantraniliprole (Cyantraniliprole) is another novel o-aminobenzamide insecticide from Dupont, following chlorantraniliprole. It has the characteristics of high efficiency, low toxicity, novel action mechanism, safety to non-target organisms, no cross resistance to the existing pesticide and the like. The cyantraniliprole has excellent control effect on piercing-sucking mouthpart pests, has wide application prospect and arouses wide attention of people.
The chemical name of cyantraniliprole is 3-bromo-1- (3-chloro-2-pyridyl) -N- { 4-cyano-2-methyl-6- [ (methylamino) carbonyl ] phenyl } -1H-pyrazole-5-carboxamide; has a chemical structural formula of
Molecular formula C19H14BrClN6O2Molecular weight 473.7. Cyantraniliprole is white powder, the melting point is 168-173 ℃, and the relative density (20 ℃) is 1.387g/cm3It is not easy to volatilize. The solubility in water (20 ℃) is 0-20 mg/L, the solubility in other solvents is 2.383g/L (methanol), 5.965g/L (acetone), 0.576g/L (toluene), 5.338g/L (dichloromethane) and 1.728g/L (acetonitrile).
The typical metabolite of cyantraniliprole in plants and animals is J9Z38, and the structural formula is:
molecular formula C19H12BrClN6O, molecular weight 457.
At present, the report about the cyantraniliprole detection method is as follows: the detection method of cyantraniliprole in crops (rice, wheat and corn), vegetables (cucumber, tomato, pakchoi, hot pepper, cowpea and lettuce), fruits (apple, grape and orange) and other plant-derived agricultural products, soil and water. However, no report is found about the detection method of cyantraniliprole and the metabolite J9Z38 in pork.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for detecting cyantraniliprole and a metabolite J9Z38 in pork, which can be used for detecting cyantraniliprole and a metabolite J9Z38 in pork and meet the requirements on accuracy, precision and sensitivity in pesticide residue analysis.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for detecting cyantraniliprole and a metabolite J9Z38 in pork comprises the following steps:
(1) extraction: weighing 2g of pork sample, placing the pork sample in a 50mL centrifuge tube, adding 2mL of 0.1% formic acid water and 20mL of extracting solution, homogenizing for 30s at 6000rpm, adding 1g of anhydrous sodium acetate and 2g of anhydrous magnesium sulfate, violently shaking for 30s, and centrifuging for 5min at 4000 rpm;
(2) purifying: transferring 10mL of extracting solution in a centrifuge tube, placing the extracting solution in a separating funnel, adding 30mL of purifying solution for the first time, violently shaking for 1min, standing for 20min, discarding the upper layer of purifying solution after the liquid in the separating funnel is layered, adding 30mL of purifying solution in the separating funnel for the second time, violently shaking for 1min, standing for 20min, discarding the upper layer of purifying solution after the liquid in the separating funnel is layered, collecting the extracting solution in the separating funnel in a flat-bottomed flask, concentrating at 40 ℃ until the volume is 5mL, and filtering through a 0.22 mu m organic needle type filter to be measured;
(3) and (3) determination: preparing 0.005, 0.01, 0.05, 0.1, 0.2, 0.5 and 1.0mg/L cyantraniliprole and J9Z38 standard solutions, respectively injecting 1 mu L of solution to obtain a response value of UPLC-MS/MS, and drawing a cyantraniliprole standard solution curve and a J9Z38 standard solution curve by concentration-peak area;
(4) when the adding concentration of cyantraniliprole in pork is set to be 0.02, 0.1 and 10.0mg/kg, an adding recovery rate test is carried out to respectively obtain the adding recovery rate and Relative Standard Deviation (RSDs) of cyantraniliprole and J9Z 38;
(5) detecting the minimum detection amount of cyantraniliprole and J9Z38 by using an ultra-high performance liquid chromatography tandem mass spectrometer;
(6) and obtaining the minimum detection concentrations of cyantraniliprole and J9Z38 in pork according to the response conditions of the cyantraniliprole and J9Z38 on an ultra performance liquid chromatography tandem mass spectrometer and the response values of samples of the cyantraniliprole in the pork and J9Z38 added according to the minimum addition concentration on the instrument, wherein the response values are all larger than 3 times of the signal-to-noise ratio of the instrument.
The extract was an acetonitrile homogenate.
The purifying liquid is n-hexane liquid.
The conditions of the ultra-high performance liquid chromatography are as follows:
a chromatographic column: waters acquity
C18(1.7μm，2.1×100mm)；
Mobile phase: acetonitrile/0.1% aqueous formic acid solution-80/20;
flow rate: 0.2 mL/min;
column temperature: 40 ℃;
sample introduction amount: 1 mu L of the solution;
the mass spectrum conditions were:
an ion source: ESI+；
Quantitative mode: an MRM mode;
capillary voltage: 4.0 KV;
flow rate of atomizing gas: 3.0L/min;
heating air flow: 10.0L/min;
interface temperature: 300 ℃;
DL temperature: 250 ℃;
heatblock temperature: 400 ℃;
flow rate of drying gas: 10L/min;
cyantraniliprole quantitative ion pair: 475.10>286.00, qualitative ion pair: 475.10> 444.10;
J9Z38 quantitative ion pair: 456.80> 188.00; and (3) qualitative ion: 456.80> 299.00.
The invention has the beneficial effects that: the invention establishes an analysis and detection method of cyantraniliprole in pork and a metabolite J9Z38 thereof; the method has the advantages that the acetonitrile homogenate extraction is adopted, the impurities such as fat, protein and the like in the pork are removed by the liquid-liquid distribution of the n-hexane, the purification and separation effect is good (the core of the invention), the pretreatment process of the method is relatively simple, the recovery rate is high, the repeatability is good, the purification and separation effect is good, the minimum detection concentration is relatively low, and the method is suitable for the analysis and detection of cyantraniliprole and the metabolite J9Z38 in the pork.
Drawings
Figure 1 is the addition recovery and relative standard deviation of cyantraniliprole and J9Z 38.
Figure 2 is a standard graph of cyantraniliprole.
Fig. 3 is a standard graph of J9Z 38.
FIG. 4 is a standard solution chromatogram of cyantraniliprole (0.1mg/L) and J9Z38(0.1 mg/L).
Detailed Description
The invention discloses a method for detecting cyantraniliprole and metabolite J9Z38 in pork, which adopts the following main instruments and chemical reagents:
ultra-high performance liquid chromatography tandem mass spectrometer UPLC-MS/MS (ultra-high performance liquid chromatography model LC-30AD, mass spectrometer model LCMS-8050, Shimadzu corporation),
SPS 402F type electronic balance: (Mettler-Tolido (Changzhou) measurement technologies, Inc.),
IKA T18 type disperser (IKA laboratory, Germany),
TD5A-WS type desk type large-capacity low-speed centrifuge (Kingnan Instrument manufacturing Co., Ltd.),
R-201 type rotary evaporator (Shanghai Shen Sheng Biotechnology Co., Ltd.),
HH-4 TYPE CONSTANT-temp. WATER BATH POT (Instrument works in south of Jiangsu jin Tan City),
SHZ-D (III) type circulating water type vacuum pump (Ongyi instruments, Inc.),
TYZD-IIA type oscillator (Jiangyan city Tianqi electronics Co., Ltd.),
Methanol (analytically pure 500mL, Tianjin Dalochi chemical reagent plant),
Ethyl acetate (analytically pure 500mL, Tianjin Dalochi chemical reagent plant),
Acetonitrile (analytically pure 500mL, Shanghai Lingfeng Chemicals Co., Ltd.),
Anhydrous sodium acetate (analytically pure 500g, Wenzhou chemical material factory),
Anhydrous magnesium sulfate (analytically pure 500g, Fuchen chemical reagent factory of Tianjin),
N-hexane (analytically pure 500mL, chemical reagents of national pharmacy group Co., Ltd.),
Cleanert MAS-Q purge tube (2mL, PSA 50mg, C)1850mg，PC 50mg，MgSO4150mg, MS-9PP0250, Techno Babon Aijiel technologies, Inc.),
Cleanert NANO CARB purification tube (150mg/1mL, model IC-NN1510-S, Tianjin Bonne Aijie technologies, Inc.),
Oasis HLB 3cc column (60mg/3mL, model WAT094226, Waters corporation),
Cleanert NH2SPE cartridges (500mg/6mL, model NH5006, Tianjin Bonne Aijier technologies, Inc.),
Acetonitrile (chromatographically pure 4L, Merck two-ply company),
Formic acid (500 mL in chromatographic purity, ROE Scientific Inc, USA),
Organic needle type filter (0.22 μm, model TQP-61322, Tianyuan science and technology company),
Syringes (2mL, changzhouyuekang medical devices, ltd).
Wherein the conditions of the apparatus are:
ultra-high performance liquid chromatography conditions:
a chromatographic column: waters acquity
C18(1.7μm，2.1×100mm)；
Mobile phase: acetonitrile/0.1% aqueous formic acid solution-80/20;
flow rate: 0.2 mL/min;
column temperature: 40 ℃;
sample introduction amount: 1 μ L.
Mass spectrum conditions:
an ion source: ESI+；
Quantitative mode: an MRM mode;
capillary voltage: 4.0 KV;
flow rate of atomizing gas: 3.0L/min;
heating air flow: 10.0L/min;
interface temperature: 300 ℃;
DL temperature: 250 ℃;
heatblock temperature: 400 ℃;
flow rate of drying gas: 10L/min;
cyantraniliprole quantitative ion pair: 475.10>286.00, qualitative ion pair: 475.10> 444.10;
J9Z38 quantitative ion pair: 456.80> 188.00; and (3) qualitative ion: 456.80> 299.00.
The specific detection operation of the invention is as follows:
extraction: sample 2g (exactly 0.01g) was weighed into a 50mL centrifuge tube, 2mL of 0.1% formic acid water and 20mL of analytically pure acetonitrile were added and homogenized (IKA T18 type disperser) at 6000rpm for 30 s. 1g of anhydrous sodium acetate and 2g of anhydrous magnesium sulfate were added and shaken vigorously for 30 s. Centrifugation (TD5A-WS model desk top high capacity low speed centrifuge) at 4000rpm for 5 min.
Methanol oscillation extraction, ethyl acetate oscillation extraction, acetonitrile oscillation extraction and acetonitrile homogenate can be used as the extracting solution of the invention, but the extraction efficiency of 4 extracting solutions is different, the extraction rate of the methanol oscillation extraction of the cyantraniliprole and the extraction rate of the J9Z38 are respectively 38 percent and 46 percent, and the extraction rate can not meet the requirement. The extraction rates of the cyantraniliprole and the J9Z38 extracted by ethyl acetate oscillation are 72% and 82% respectively, and the extraction rates can meet the requirements. The extraction rates of acetonitrile oscillation extraction of cyantraniliprole and J9Z38 are respectively 71% and 85%, and the extraction rates can meet the requirements. The extraction rate of cyanogenamide bromide and J9Z38 extracted by acetonitrile homogenate is 82% and 89%, and the extraction rate can meet the requirement. The extraction method comprises 3 conditions of ethyl acetate oscillation extraction, acetonitrile oscillation extraction and acetonitrile homogenate extraction, wherein the extraction rates of cyantraniliprole and J9Z38 can meet requirements, factors such as the extraction rate, the extraction time and the like are comprehensively considered, and the acetonitrile homogenate extraction is the optimal extraction condition, so that the acetonitrile homogenate extraction is determined to be used as the extraction method of cyantraniliprole and J9Z38 in pork.
Purifying: accurately transferring 10mL of acetonitrile in a centrifuge tube, placing the centrifuge tube in a separating funnel, adding 30mL of normal hexane for the first time, violently shaking for 1min, and standing for 20 min. And after the liquid in the separating funnel is layered, removing the upper n-hexane layer. Adding 30mL of n-hexane into the separating funnel for the second time, shaking vigorously for 1min, and standing for 20 min. After the liquid in the separating funnel is separated, the upper n-hexane layer is discarded, the acetonitrile in the separating funnel is collected in a flat-bottom flask, concentrated and dried at 40 ℃ (R-201 type rotary evaporator), the volume is adjusted to 5mL by chromatographic pure acetonitrile, and the acetonitrile passes through a 0.22 mu m organic needle type filter (model is TQP-61322) to be measured.
Comparison of NH when selected for cleaning2SPE cartridge, HLB cartridge, Cleanert MAS-Q purification tube (2mL, C)1850mg，PSA 50mg，PC 50mg，MgSO4150mg), an IC-NN1510-S type clean NANO CARB purification tube (150mg/1mL), n-hexane liquid-liquid distribution and the like, on the purification effect of cyantraniliprole and J9Z38 in pork. The result shows that the NH is cleaned NH of NH5006 type2After purification by SPE cartridge (500mg/6mL), the recovery rates of cyantraniliprole and J9Z38 are 53% and 66%, respectively, and the recovery rate is not up to the requirement. After the purification by WAT094226 type Oasis HLB 3cc column (60mg/3mL), the recovery rates of cyantraniliprole and J9Z38 are 47% and 70%, respectively, and the recovery rates can not meet the requirements. Passing through MS-9PP0250 type Cleanert MAS-Q purification tube (2mL, PSA 50mg, C)1850mg，PC 50mg，MgSO4150mg), the recovery rates of cyantraniliprole and J9Z38 are 72% and 79%, respectively, and the recovery rates can meet the requirements. After being purified by an IC-NN1510-S type Cleanert NANO CARB purifying tube (150mg/1mL), the recovery rates of cyantraniliprole and J9Z38 are 67 percent and 74 percent respectively, and the recovery rates can not meet the requirements. After n-hexane liquid-liquid distribution and purification, the recovery rates of cyantraniliprole and J9Z38 are respectively 105% and 91%, and the recovery rates can meet the requirements; the purified liquid is colorless, the effect of removing impurities is good, the recovery rate is comprehensively considered,Impurity removal effect, operation process and other factors, and the distribution of the n-hexane liquid is the optimal purification condition, so that the distribution of the n-hexane liquid is determined as a purification method of cyantraniliprole and J9Z38 in pork.
Preparing 0.005, 0.01, 0.05, 0.1, 0.2, 0.5 and 1.0mg/L cyantraniliprole and J9Z38 standard solutions by using chromatographic pure acetonitrile, injecting 1 mu L of the standard solutions respectively to obtain a response value of UPLC-MS/MS, drawing a curve of the standard solution of the cyantraniliprole by using concentration-peak area, and obtaining a regression equation of the curve, wherein the regression equation is that y is 9835407.97x +24039.88(R is shown in figure 2)20.9999); standard solution curve of J9Z38, see fig. 3, with regression equation of y 1601429.98x +2065.58 (R)2＝1.0000)。
Cyantraniliprole, J9Z38, was set to 3 addition levels (0.02, 0.1 and 10mg/kg) in the pork samples, with 5 replicates per addition level, according to the response of cyantraniliprole, J9Z38 on an ultra performance liquid chromatography tandem mass spectrometer (UPLC-MS/MS).
The addition recovery test was performed according to the extraction, purification and measurement procedures described above. The added recovery and Relative Standard Deviations (RSDs) of cyantraniliprole, J9Z38, were obtained for the pork samples, see figure 1.
As can be seen from fig. 1, when cyantraniliprole was added to pork at concentrations of 0.02, 0.1 and 10.0mg/kg, the average recovery rates were 107%, 102% and 96%, respectively, and the relative standard deviations were 3.7%, 3.5% and 3.6%, respectively. The average recovery rates of the J9Z38 were 93%, 88% and 93% and the relative standard deviations were 3.1%, 4.0% and 5.3% respectively when the pork was added at concentrations of 0.02, 0.1 and 10.0 mg/kg.
The minimum detection amount of the ultra performance liquid chromatography tandem mass spectrometer (UPLC-MS/MS) on cyantraniliprole and J9Z38 is 5 x 10 < -12 > g.
According to the response conditions of cyantraniliprole and J9Z38 on an ultra performance liquid chromatography tandem mass spectrometer, and the response values of samples of cyantraniliprole and J9Z38 with the lowest addition concentration of 0.02mg/kg in pork on the instrument are all larger than 3 times of the signal-to-noise ratio of the instrument, the following are obtained: the minimum detection concentrations of cyantraniliprole and J9Z38 in pork are both 0.02 mg/kg.
The invention establishes an analysis and detection method for cyantraniliprole in pork and a metabolite J9Z38 thereof, wherein the cyantraniliprole and the metabolite J9Z38 are in a good linear relation within a concentration range of 0.005-1.0 mg/L; the average recovery rate of cyantraniliprole in pork is 96-101%, and the relative standard deviation is 5.0-13.8%. The average recovery rate of J9Z38 in pork is 93-97%, and the relative standard deviation is 2.9-11.0%. The minimum detection concentrations of cyantraniliprole and J9Z38 in pork are both 0.02mg/kg, the method is simple and convenient to operate, accurate and reliable, can meet the requirement of pesticide residue analysis, and can be used for rapid detection of a large number of samples.
Claims (1)
1. The detection method of cyantraniliprole and metabolite J9Z38 in pork is characterized by comprising the following steps:
(1) extraction: weighing 2g of pork sample, placing the pork sample in a 50mL centrifuge tube, adding 2mL of 0.1% formic acid water and 20mL of extracting solution, homogenizing for 30s at 6000rpm, adding 1g of anhydrous sodium acetate and 2g of anhydrous magnesium sulfate, violently shaking for 30s, and centrifuging for 5min at 4000 rpm;
(2) purifying: transferring 10mL of extracting solution in a centrifuge tube, placing the extracting solution in a separating funnel, adding 30mL of purifying solution for the first time, violently shaking for 1min, standing for 20min, discarding the upper layer of purifying solution after the liquid in the separating funnel is layered, adding 30mL of purifying solution in the separating funnel for the second time, violently shaking for 1min, standing for 20min, discarding the upper layer of purifying solution after the liquid in the separating funnel is layered, collecting the extracting solution in the separating funnel in a flat-bottomed flask, concentrating at 40 ℃ until the volume is 5mL, and filtering through a 0.22 mu m organic needle type filter to be measured;
(3) and (3) determination: preparing 0.005, 0.01, 0.05, 0.1, 0.2, 0.5 and 1.0mg/L cyantraniliprole and J9Z38 standard solutions, respectively injecting 1 mu L of solution to obtain a response value of UPLC-MS/MS, and drawing a curve of the cyantraniliprole standard solution by using a concentration-peak area;
(4) the adding concentration of cyantraniliprole and metabolite J9Z38 in pork is set to be 0.01, 0.2 and 8.0mg/kg, and an adding recovery rate test is carried out to respectively obtain the adding recovery rate and the relative standard deviation of cyantraniliprole and J9Z 38;
(5) detecting the minimum detection amount of cyantraniliprole and J9Z38 by using an ultra-high performance liquid chromatography tandem mass spectrometer;
(6) according to the response conditions of cyantraniliprole and J9Z38 on an ultra performance liquid chromatography tandem mass spectrometer, and the response values of samples, added according to the lowest adding concentration, of cyantraniliprole and J9Z38 in pork on the instrument are both larger than 3 times of the signal-to-noise ratio of the instrument, so that the lowest detection concentrations of cyantraniliprole and J9Z38 in pork are obtained;
the extract is an acetonitrile homogenate;
the purifying liquid is n-hexane liquid;
the chromatographic conditions of the ultra-high performance liquid chromatography tandem mass spectrometer are as follows:
a chromatographic column: waters acquity
BEH C18，1.7μm，2.1×100mm；
Mobile phase: acetonitrile/0.1% aqueous formic acid solution-80/20;
flow rate: 0.2 mL/min;
column temperature: 40 ℃;
sample introduction amount: 1 mu L of the solution;
the mass spectrum conditions of the ultra-high performance liquid chromatography tandem mass spectrometer are as follows:
an ion source: ESI+；
Quantitative mode: an MRM mode;
capillary voltage: 4.0 KV;
flow rate of atomizing gas: 3.0L/min;
heating air flow: 10.0L/min;
interface temperature: 300 ℃;
DL temperature: 250 ℃;
heatblock temperature: 400 ℃;
flow rate of drying gas: 10L/min;
cyantraniliprole quantitative ion pair: 475.10>286.00, qualitative ion pair: 475.10> 444.10; J9Z38 quantitative ion pair: 456.80> 188.00; and (3) qualitative ion: 456.80> 299.00.
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