ursodeoxycholic acid-CAD Detector test report

ursodeoxycholic acid, the chemical name is 3a,7β-Dihydroxy-5β-cholestane-24-Acid is an organic compound, odorless and bitter. It is used medically to increase bile acid secretion, change bile composition, reduce cholesterol and cholesterol lipids in bile, and help the cholesterol in gallstones gradually dissolve.CAS Login number: 128-13-2;EINECS Login number: 204-879-3;Chinese name: ursodeoxycholic acid;Molecular weight: 392.572.

Chinese Pharmacopoeia 2020 version,ursodeoxycholic acid Thin layer chromatography is used for the relevant substances, and the titration method is used for content determination. This article develops an electrospray detection method to improve the applicability and repeatability of the original method, while improving the detection limit of impurities and improving the quality control level of the drug.

Charged Aerosol Detector (CAD)(charged aerosol detector,CAD) is a new general-purpose detector developed in recent years. Its detection has nothing to do with the molecular structure of the substance being measured, and the substance being measured does not need to be ionized. It can be used as long as the substance being measured is a semi-volatile or non-volatile compound.CAD detection. At the same time,CAD It is a mass-sensitive detector. The response value of the measured substance is determined by the absolute mass of the sample being tested. As long as the absolute mass of the sample being tested is consistent, the measured response value will basically be the same, and a lower detection limit and higher sensitivity can be obtained.

1, instruments and materials

Instruments:Agilent1200 liquid chromatograph+Charged Aerosol Detector (CAD)(INSTRUMAX, Model: CADetector a1)

Reagents: ammonium acetate, pure water (Watson's distilled water), methanol (chromatography grade), formic acid (analytical grade)

Sample:UDA21 and UDP2451(Friendly provided by user teacher,UDP2451 for crude products).

2, methods and results

2.1 Chromatographic conditions

Column:ODS Hypersil 125✖4mm,3μm Column temperature:40℃ Flow rate:0.8mL/min

Injection volume:10μL

Mobile phase A:5mm ol/L ammonium acetate+0.1%Formic acid aqueous solution mobile phase B: methanol

Gradient conditions:

CAD Conditions:

Instrument model:INSTRUMAX CADetector a1

Drift tube temperature:40℃

Atomized air flow:3L/min

Polarization current:1μA

Polarized airflow:1L/min

2.2 Sample preparation

Thinner: Methanol - Liquidity A (70:30)

Sample weighing approx.20mg, set 10mL Volumetric flask, after dissolving it in methanol, use 70%Dilute the diluent to the mark to obtain (sample concentration: approx.2mg/mL).

UDA21 Sample preparation 1%Control sample (sample concentration:20μg/mL)

2.3 Experimental results

Note: Each sample is equipped with a partial enlargement of the chromatogram.

3, experimental conclusion

CAD Yes ursodeoxycholic acid The detection response is good; impurities can be better detected;

Charged Aerosol Detector (CAD) can do ursodeoxycholic acid Process optimization, quality control, etc. provide testing data support.HPLC-CAD The method is simple to operate, highly specific, and highly sensitive, and can be used as ursodeoxycholic acid quality control and evaluation methods.