Analysis method for measuring dimethyl sulfate in pyraclostrobin by gas chromatography-mass spectrometry
A technology of dimethyl sulfate and pyraclostrobin, which is applied in the field of analysis and can solve the problems of unchecked analysis and detection of dimethyl sulfate
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Embodiment 1
[0034] Embodiment 1, standard solution preparation
[0035] Weigh about 0.020g (accurate to 0.02mg) dimethyl sulfate standard sample, put it in a 50mL volumetric flask, dissolve it with dichloromethane, dilute to volume, and shake well. Accurately draw 5.00mL of the solution, and put it in a 100mL volumetric flask , dilute to volume with dichloromethane and shake well. Then accurately draw 5.00 mL of the standard stock solution, place it in a 250 mL volumetric flask, dilute to volume with dichloromethane, shake well, and prepare the standard parent drug with a mass concentration of 0.4 μg / mL.
Embodiment 2
[0036] Embodiment 2, standard curve:
[0037] Accurately pipette 4.00, 6.00, 10.00, 12.00, 15.00 and 20.00mL of 0.4μg / mL standard parent drug to prepare a standard working curve solution, and use the method of gas chromatography to draw the standard with the mass concentration as the abscissa and the peak area as the ordinate. curve to get the linear regression equation.
[0038] y=19284067.2149x-28.6500, R 2 = 0.9999.
Embodiment 3
[0039] The mensuration of dimethyl sulfate content in embodiment 3, sample
[0040] Weigh about 1.5g of the sample (accurate to 0.2mg), put it in a 25mL volumetric flask, add dichloromethane to dissolve, make up to volume, and shake well.
[0041] Using GC method, record the peak area of dimethyl sulfate in the sample, and substitute the peak area into the standard curve linear regression equation to calculate the content of dimethyl sulfate.
[0042] Adopt gas chromatography-mass spectrometry (quadrupole mass analyzer) analysis condition is as follows:
[0043] Chromatographic column: HP-5MS cross-linked capillary column, 30m×0.25mm(i.d.)×0.25μm
[0044] Column temperature:
[0045] Carrier gas (He): 1.2mL / min;
[0046] Vaporization temperature: 250°C;
[0047] Ion source: EI, 70eV;
[0048] Ion source temperature: 230°C;
[0049] Quadrupole mass analyzer temperature: 150°C;
[0050] Split ratio: 10:1;
[0051] Detection mode: single ion scan m / z 95;
[0052] Inj...
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