Method for measuring tert-butyl hydrazine hydrochloride by use of pre-column derivatization-high performance liquid chromatography

Abstract

The invention discloses a method for measuring tert-butyl hydrazine hydrochloride by use of pre-column derivatization-high performance liquid chromatography. The method comprises the following steps: by taking benzaldehyde as a derivatization reagent, reacting under the PH of 5.0 and at 30 DEG C for 90 minutes; employing an Elitehplc 1201 high performance liquid chromatograph and an ultraviolet variable detector; adopting a Hypersil BDS C18 (5mu m, 4.6*250mm) chromatographic column; measuring under the conditions of a column temperature within the range of 25-35 DEG C, a mobile phase being 70%-100%(v / v) methanol aqueous solution, a flow velocity within the range of 0.8-1.2mL / min, a detection wavelength of 298nm and a sample size of 20mu L, and recording a peak area; drawing a tert-butyl hydrazine hydrochloride concentration-tert-butyl hydrazine hydrochloride derivative peak area standard curve by use of an external standard method and obtaining a standard curve regression equation; next, calculating the content of the tert-butyl hydrazine hydrochloride. The method is capable of eliminating the interference of hydrazine hydrochloride in the content measurement process and accurately quantitating the tert-butyl hydrazine hydrochloride. The method is complete in derivatization reaction, simple and easy to operate, convenient and reliable, and easy to popularize, and has relatively high accuracy and precision.

Description

technical field

[0001] The invention belongs to the technical field of analysis, and relates to a quantitative analysis method for tert-butylhydrazine hydrochloride, in particular to a method for determining tert-butylhydrazine hydrochloride by pre-column derivatization-high performance liquid chromatography. Background technique

[0002] Tert butyl hydrazine hydrochloride, also known as tert butyl hydrazine hydrochloride, is an important pesticide intermediate; , Halofenozide, Methoxyfenozide, Chromafenozide and Pyridben are important raw materials for insecticides. Because tert-butylhydrazine hydrochloride introduces more hydrazine hydrochloride in the production process and is not easy to separate. Therefore, the quality control of tert-butylhydrazine hydrochloride directly affects the quality of the synthetic product.

[0003] There are three main methods for the determination of tert-butylhydrazine hydrochloride currently reported: (1) iodometric method (redox titrati...

Examples

Embodiment 1

[0038] Preparation of reference substance solution: Accurately weigh 0.1000g (accurate to 0.0001g) of tert-butylhydrazine hydrochloride reference substance, put it in a 10ml volumetric flask, dissolve it with ultrapure water and adjust the volume to the mark. Prepared as a 10mg / mL reference substance solution.

[0039] Preparation of sample solution: Accurately weigh 0.1100g (accurate to 0.0001g) of tert-butylhydrazine hydrochloride sample, put it in a 10ml volumetric flask, dissolve it with ultrapure water and adjust the volume to the mark. Prepare a sample solution containing about 10 mg / mL of tert-butylhydrazine hydrochloride.

[0040] Preparation of derivatization reagent: Weigh 0.40g of benzaldehyde (accurate to 0.01g), put it in a 10ml volumetric flask, dissolve it with absolute ethanol and set the volume to the mark. Prepare a derivatization reagent containing benzaldehyde 40mg / mL.

[0041] Drawing of the standard curve: Accurately measure 0.3, 0.4, 0.5, 0.6, 0.7mL o...

Embodiment 2

[0055] The preparation of reference substance solution is the same as implementation example one.

[0056] The preparation of the sample solution is the same as that of Example 1.

[0057] The preparation of the derivatization reagent is the same as that of Example 1.

[0058] Chromatographic conditions: Elite 1201 high performance liquid chromatography, UV variable detector; Hypersil BDS C18 (5μm, 4.6×250mm) chromatographic column; column temperature 30°C; mobile phase is methanol: water = 80:20; flow rate is 1.0 mL / min; the detection wavelength is 298nm; the injection volume is 20μL (quantitative loop).

[0059] The drawing of standard curve is the same as implementation example one. The experimental results are shown in Table 3.

[0060] Table 3 Standard curve determination experimental results.

[0061]

[0062] According to the above experimental results, a standard curve of tert-butylhydrazine hydrochloride concentration-tert-butylhydrazine hydrochloride derivati...

Embodiment 3

[0073] The preparation of reference substance solution is the same as implementation example one.

[0074] The preparation of the sample solution is the same as that of Example 1.

[0075] The preparation of the derivatization reagent is the same as that of Example 1.

[0076] Chromatographic conditions: Elite 1201 high performance liquid chromatograph, UV variable detector; Hypersil BDS C18 (5μm, 4.6×250mm) chromatographic column; column temperature 35°C; mobile phase is methanol: water = 80:20; flow rate is 1.1 mL / min; the detection wavelength is 298nm; the injection volume is 20μL (quantitative loop).

[0077] The drawing of standard curve is the same as implementation example one. The experimental results are shown in Table 5.

[0078] Table 5 Standard curve drawing experimental results.

[0079]

[0080] According to the above experimental results, a standard curve of tert-butylhydrazine hydrochloride concentration-tert-butylhydrazine hydrochloride derivative peak...

technical field

[0001] The invention belongs to the technical field of analysis, and relates to a quantitative analysis method for tert-butylhydrazine hydrochloride, in particular to a method for determining tert-butylhydrazine hydrochloride by pre-column derivatization-high performance liquid chromatography. Background technique

[0002] Tert butyl hydrazine hydrochloride, also known as tert butyl hydrazine hydrochloride, is an important pesticide intermediate; , Halofenozide, Methoxyfenozide, Chromafenozide and Pyridben are important raw materials for insecticides. Because tert-butylhydrazine hydrochloride introduces more hydrazine hydrochloride in the production process and is not easy to separate. Therefore, the quality control of tert-butylhydrazine hydrochloride directly affects the quality of the synthetic product.

[0003] There are three main methods for the determination of tert-butylhydrazine hydrochloride currently reported: (1) iodometric method (redox titrati...

Examples

Embodiment 1

[0038] Preparation of reference substance solution: Accurately weigh 0.1000g (accurate to 0.0001g) of tert-butylhydrazine hydrochloride reference substance, put it in a 10ml volumetric flask, dissolve it with ultrapure water and adjust the volume to the mark. Prepared as a 10mg / mL reference substance solution.

[0039] Preparation of sample solution: Accurately weigh 0.1100g (accurate to 0.0001g) of tert-butylhydrazine hydrochloride sample, put it in a 10ml volumetric flask, dissolve it with ultrapure water and adjust the volume to the mark. Prepare a sample solution containing about 10 mg / mL of tert-butylhydrazine hydrochloride.

[0040] Preparation of derivatization reagent: Weigh 0.40g of benzaldehyde (accurate to 0.01g), put it in a 10ml volumetric flask, dissolve it with absolute ethanol and set the volume to the mark. Prepare a derivatization reagent containing benzaldehyde 40mg / mL.

[0041] Drawing of the standard curve: Accurately measure 0.3, 0.4, 0.5, 0.6, 0.7mL o...

Embodiment 2

[0055] The preparation of reference substance solution is the same as implementation example one.

[0056] The preparation of the sample solution is the same as that of Example 1.

[0057] The preparation of the derivatization reagent is the same as that of Example 1.

[0058] Chromatographic conditions: Elite 1201 high performance liquid chromatography, UV variable detector; Hypersil BDS C18 (5μm, 4.6×250mm) chromatographic column; column temperature 30°C; mobile phase is methanol: water = 80:20; flow rate is 1.0 mL / min; the detection wavelength is 298nm; the injection volume is 20μL (quantitative loop).

[0059] The drawing of standard curve is the same as implementation example one. The experimental results are shown in Table 3.

[0060] Table 3 Standard curve determination experimental results.

[0061]

[0062] According to the above experimental results, a standard curve of tert-butylhydrazine hydrochloride concentration-tert-butylhydrazine hydrochloride derivati...

Embodiment 3

[0073] The preparation of reference substance solution is the same as implementation example one.

[0074] The preparation of the sample solution is the same as that of Example 1.

[0075] The preparation of the derivatization reagent is the same as that of Example 1.

[0076] Chromatographic conditions: Elite 1201 high performance liquid chromatograph, UV variable detector; Hypersil BDS C18 (5μm, 4.6×250mm) chromatographic column; column temperature 35°C; mobile phase is methanol: water = 80:20; flow rate is 1.1 mL / min; the detection wavelength is 298nm; the injection volume is 20μL (quantitative loop).

[0077] The drawing of standard curve is the same as implementation example one. The experimental results are shown in Table 5.

[0078] Table 5 Standard curve drawing experimental results.

[0079]

[0080] According to the above experimental results, a standard curve of tert-butylhydrazine hydrochloride concentration-tert-butylhydrazine hydrochloride derivative peak...

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