Method for rapidly detecting content of conjugated estrogens in pregnant mare urine by utilizing near infrared spectroscopy

A near-infrared spectroscopy and estrogen-binding technology is applied in the field of rapid detection of the content of conjugated estrogen in the urine of pregnant horses, which can solve the problems of cumbersome operation, lag in analysis results, time-consuming and labor-intensive, etc., and achieves high detection accuracy and high accuracy. , the effect of easy operation

CN111579523APending Publication Date: 2020-08-25XINJIANG NUZILINE BIO PHARMA CO LTD +1
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
Publication Date
2020-08-25

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Abstract

The invention relates to the technical field of chemical detection, and provides a method for rapidly detecting the content of conjugated estrogens in pregnant mare urine by utilizing near infrared spectroscopy. Aiming at different conjugated estrogen components, a quantitative analysis and correction model of each conjugated estrogen is established by adopting a partial least square method through preprocessing and selecting characteristic spectral bands. Compared with an HPLC (high performance liquid chromatography) method, the near infrared spectroscopy provided by the invention is simpler,more convenient and quicker to operate, is suitable for content determination of large-batch samples, can meet the requirements on large-scale sample information acquisition in industrial production,and has important significance on the drug production process and stability controllability of a terminal product. Results of the embodiment show that the method provided by the invention is relatively high in detection accuracy, relative deviation between a predicted value obtained by adopting the method provided by the invention and a real value is less than 15%, and accuracy is relatively high.
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Description

technical field

[0001] The invention relates to the technical field of chemical detection, in particular to a method for rapidly detecting the content of conjugated estrogen in urine of pregnant horses by using near-infrared spectroscopy. Background technique

[0002] Conjugated estrogens are a natural blend of estrogens extracted from the urine of pregnant horses. Clinically, it is mainly used for hormone replacement therapy to relieve clinical symptoms caused by estrogen deficiency. The average content of estrogen rich in urine per liter of pregnant horse is 70-130mg, and each pregnant horse can form 5-100g of estrogen during pregnancy.

[0003] However, in the actual production process of pregnant horse urine, due to the constraints of many aspects in the process of collecting urine, the detection is mostly performed offline and analyzed afterwards. Therefore, there are many defects in the detection process. For example, the degradation of the quality control index comp...

Examples

Embodiment 1

[0087] Experimental instruments and reagents: at room temperature (15-30 ° C), using Antaris MX Fourier near-infrared process analyzer (Thermo Fisher Scientific Corporation, the United States, light source: tungsten halogen lamp, detector: InGaAs detector); Waters 2695 high performance liquid chromatography (including Alliance control panel, ultraviolet detector PDA-2998, chromatography workstation Empower2).

[0088] Experimental materials: Mixed standards of estrone sodium sulfate, equilin sulfate sodium and 17α-dihydroequilin sodium sulfate; pregnant horse urine.

[0089] (1) Preparation of the test solution: take 25mL of pregnant horse urine and place it in a centrifuge tube, after centrifugation (centrifugation speed is 4000r / min, centrifugation time 15min), accurately absorb 5mL of centrifuged supernatant and place it in 100mL Add 50mL of water to the measuring bottle, add 1mL of 1mol / L hydrochloric acid solution, shake rapidly for 2 minutes, adjust the pH value to 7.5 w...

Embodiment 2

[0139] Need testing solution is provided according to the method of embodiment 1, the true value content of estrone sodium sulfate in need testing solution is tested according to the high performance liquid chromatography condition of embodiment 1;

[0140] The test solution is scanned by near-infrared spectrum, and the spectral data of the test solution is collected. The near-infrared spectrometer (concentrating NIR1500 spectrometer) is based on the principle of grating scanning spectroscopy. The light source: tungsten halogen lamp; : InGaAs detector, resolution: 8cm -1 ; Number of scans: 32 times; optical path 1mm.

[0141] Each pregnant horse urine sample was scanned 4 times, and each measurement took an average of 4 seconds, and the average value was taken as the spectral data.

[0142] Preprocess the spectral data, and select the modeling band, then use the correlation coefficient method to select the band selection method of the wavelength range, and use the partial lea...