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Method for synchronous determination of content of triazole chiral pesticide enantiomers

A technology for enantiomers and triazoles, which is applied in the field of simultaneous determination of the enantiomer content of triazoles chiral pesticides, can solve the problem of the inability to achieve simultaneous separation of multiple chiral pesticide enantiomers, high-sensitivity detection, and influence methods. selectivity and low sensitivity

Active Publication Date: 2012-02-15
INST OF QUALITY STANDARD & TESTING TECH FOR AGRO PROD OF CAAS
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Problems solved by technology

Since the UV detector is a general-purpose detector, it is easily interfered by the sample matrix during the determination of the sample and affects the selectivity of the method. At the same time, the sensitivity of the detector is relatively low, so it is impossible to achieve the enantiometry of various chiral pesticides. Simultaneous separation and high-sensitivity detection of bulk

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  • Method for synchronous determination of content of triazole chiral pesticide enantiomers
  • Method for synchronous determination of content of triazole chiral pesticide enantiomers
  • Method for synchronous determination of content of triazole chiral pesticide enantiomers

Examples

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Embodiment 1

[0104] Example 1, Characteristic Separation of Enantiomers of Triazole Chiral Pesticides

[0105] 1. Investigation of Enantiomeric Separation Conditions

[0106] A Phenomenex Lux Cellulose-1 chiral chromatography column packed with cellulose-3,5-dimethylphenylcarbamate chiral stationary phase with a particle size of 3 μm was used, and acetonitrile / water and methanol / water were used as mobile phases In reversed-phase liquid chromatography, the enantiomers of the above nine chiral pesticides were resolved with a flow rate of 0.3mL / min and a detection wavelength of 220nm, and the volume ratios of acetonitrile / water were 90 / 10, 80 / 20 , 70 / 30, 60 / 40, 50 / 50, and methanol / water volume ratios of 90 / 10, 85 / 15, 80 / 20, 75 / 25, 70 / 30, respectively, the impact on enantiomeric resolution, the results See Table 4 and Table 5.

[0107] Table 4. Chromatographic separation parameters of enantiomers of triazole chiral pesticides

[0108]

[0109] Table 5, cyproconazole enantiomeric chromato...

Embodiment 2、 3

[0128] Embodiment 2, synchronous determination of triazole chiral pesticide enantiomer content

[0129] 1. Synchronous separation of enantiomers and establishment of LC / MS / MS analysis method

[0130] The standard solutions of 9 kinds of chiral pesticides were used to optimize the mass spectrometry parameters on the API2000 triple quadrupole tandem mass spectrometer, including the selected multiple reaction monitoring (MRM) quantitative and qualitative ion pairs, collision energy (CE), solution Cluster voltage (DP), etc., the optimization results are shown in Table 2.

[0131] Table 2. Mass Spectrometry Detection Conditions

[0132]

[0133] Under these conditions, it was combined with liquid chromatography, and the chromatographic separation conditions of 9 chiral pesticide enantiomers were optimized by using acetonitrile / water constant ratio and gradient elution procedures. For better enantiomeric separation and chromatographic peak shape, the optimal elution conditions ar...

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Abstract

The invention discloses a method for synchronous determination of the content of triazole chiral pesticide enantiomers. According to the method, the technology of accelerated solvent extraction is used to treat a soil sample, an online polarimetric optical detector is used to determine the eluting sequence of the enantiomers, and the methods of reverse phase liquid chromatography with a chiral stationary phase and triple quadruple tandem mass spectrometry are utilized for synchronous determination of enantiomers of nine triazole chiral pesticides, namely, hexaconazole, flutriafol, diniconazole, cyproconazole, tetraconazole, epoxiconazole, myclobutanil, fenbuconazole and triadimefon; the detection limit of the method is as low as 0.5 to 1.0 mu g / kg.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and the technical field of pesticide residue detection, and relates to a method for synchronously measuring the enantiomer content of triazole chiral pesticides. Background technique [0002] There may be huge differences in the activity, toxicity, absorption, degradation, metabolism and elimination of chiral pesticide enantiomers in the natural environment and organisms. For example, the biological activities of the two enantiomers are often different. It is even diametrically opposite: that is, one enantiomer has a good control effect on diseases and insect pests, while the other enantiomer has little or no effect, and may even produce strong toxic side effects. Affected by market demand, economic benefits and environmental protection factors, people have also begun to use a single active enantiomer or increase the content of a certain active enantiomer to improve the effect of pest control a...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 邱静杨曙明于红侠
Owner INST OF QUALITY STANDARD & TESTING TECH FOR AGRO PROD OF CAAS
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