Method for detecting acetylcysteine and related substances thereof

Abstract

The invention relates to a method for detecting acetylcysteine and related substances thereof. The method adopts a high performance liquid chromatography, wherein the chromatographic condition is that styrene-divinylbenzene copolymer type superpolymer chromatographic column, namely MKF-RP-MH is 4 to 10 mu meters and (100-300)*(8.0-4.0) millimeters (I.D.); the volume ratio of phosphate buffer (pH is between 2 and 5) with mobile phase compositions of 0.01-0.05 mol / L to acetonitrile is 80-95:20-5; the flowing speed is between 0.8 and 1.2 mL / min; the detecting wavelength detected by an ultraviolet detector is 210nm; and the sample size is between 10 and 20 mu liters. The method does not use ionpairreagent, overcomes the defects that ODS column detecting method does not have acid resistance or low organic phase resistance when detecting the acetylcysteine.

Description

(1) Technical field [0001] The invention relates to a high performance liquid chromatography (HPLC) detection method, in particular to a chromatographic column packed with a high polymer (ie, styrene-divinylbenzene copolymer, PS-DVB) chromatographic medium as a separation carrier to detect acetyl Analysis and detection method of cysteine ​​and its related substances. (2) Background technology [0002] Acetylcysteine ​​is an essential amino acid for the synthesis of glutathione, an antioxidant containing sulfhydryl groups, and is used for the treatment of acute and chronic bronchitis and other lung diseases caused by sticky sputum. Acetylcysteine ​​can also be used in the treatment of HIV-infected patients to improve the physiology and immune function of patients with cysteine ​​deficiency caused by the virus. [0003] Acetylcysteine ​​is easy to introduce related substances such as L-cystine, L-cysteine, N,N'-diacetylcystine and N,S-diacetylcystine during the production pro...

AI Technical Summary

Problems solved by technology

At present, the pharmacopoeias of various countries have strict regulations on the related substances of acetylcysteine. Among them, the 2005 edition of "Chinese Pharmacopoeia" uses the iodometric method to determine the content of acetylcysteine, but does not stipulate related substances; "The 28 edition uses HPLC and ODS column, with phenylalanine as the internal standard substance, to measure the content of acetylcysteine, also does not stipulate related substances; "British Pharmacopoeia" 2003 edition uses ODS column, utilizes ion Chromatographic separation of acetylcysteine ​​and its related substances has a good separation effect, but the ion-pairing reagent (sodium heptanesulfonate) used in the mobile phase is relatively expensive, the detection cost is high, and the pH of the mobile phase is low , will also affect the service life of the chromatographic column; in addition, the method of "Chinese National Drug Standards" (implemented on January 1, 2007), the standard number is: WS1-(X-261)-2003Z-2006) is the same as that of "British Pharmacopoeia" 2003 The method described in the version is basically the same, and sodium heptanesulfonate is also needed; "European Pharmacopoeia" 52 edition uses ODS column, utilizes ion suppression chromatography to analyze acetylcysteine ​​and its related substances, and the mobile phase system used in this method Relatively simple, but the proportion of organic phase in the mobile phase of this analysis method is low (only 3%), which is lower than the lower limit of ordinary ODS columns (the lowest proportion of organic phase is 5%), and the pH value of the mobile phase is also low, long-term use have an effect on the lifetime of the column