CN-121978224-A - HPLC-ELCD method for simultaneously detecting calcium gluconate, zinc gluconate and lysine hydrochloride and application thereof

Abstract

The invention relates to the technical field of substance detection, and particularly discloses an HPLC-ELCD method for simultaneously detecting calcium gluconate, zinc gluconate and lysine hydrochloride and application thereof. In the HPLC-ELCD method for simultaneously detecting calcium gluconate, zinc gluconate and lysine hydrochloride, a cation exchange chromatographic column is adopted for isocratic elution of a sample to be detected, a mobile phase is a methylsulfonic acid-oxalic acid solution, the concentration of methylsulfonic acid in the methylsulfonic acid-oxalic acid solution is 0.002mol/L-0.004mol/L, and the concentration of oxalic acid is 0.12g/L-0.18g/L. The method has the advantages of high separation efficiency, good selectivity, high detection sensitivity and strong operability.

Inventors

• TAO XIUMEI
• WANG DONG
• WANG JUAN
• XU YANHONG

Assignees

• 北京诺康达医药科技股份有限公司

Dates

Publication Date

20260505

Application Date

20241031

Claims (10)

1. 1. An HPLC-ELCD method for simultaneously detecting calcium gluconate, zinc gluconate and lysine hydrochloride is characterized in that a cation exchange chromatographic column is adopted for isocratic elution of a sample to be detected, a mobile phase is a methylsulfonic acid-oxalic acid solution, the concentration of methylsulfonic acid in the methylsulfonic acid-oxalic acid solution is 0.002mol/L-0.004mol/L, and the concentration of oxalic acid is 0.12g/L-0.18g/L.
2. 2. The HPLC-ELCD method of claim 1, wherein the concentration of methylsulfonic acid in the mobile phase is 0.003mol/L and the concentration of oxalic acid is 0.15g/L.
3. 3. HPLC-ELCD method according to claim 1 or 2, characterized in that the chromatographic column is of model Dionex IonPac TM SCS1.
4. 4. A HPLC-ELCD method according to any one of claims 1-3, characterized in that the column temperature is 30 ± 5 ℃, the flow rate is 1 ± 0.2ml/min and the sample loading is 5-25 μl.
5. 5. Use of the HPLC-ELCD method of any one of claims 1-4 for detecting calcium zinc gluconate in an oral solution.
6. 6. A method for simultaneously detecting calcium gluconate, zinc gluconate and lysine hydrochloride in a calcium zinc gluconate oral solution, wherein the detection of a sample of the calcium zinc gluconate oral solution is performed by the HPLC-ELCD method according to any one of claims 1 to 4.
7. 7. The method of claim 6, wherein the sample is diluted with water prior to detection.
8. 8. The method according to claim 6 or 7, further comprising the step of quantifying the calcium gluconate, zinc gluconate and/or lysine hydrochloride by an external standard method after detecting the calcium gluconate, zinc gluconate and/or lysine hydrochloride in the sample.
9. 9. Use of the method according to any one of claims 6-8 for quality monitoring of calcium zinc gluconate oral solutions.
10. 10. The use according to claim 9, wherein the quality monitoring means qualitative and/or quantitative monitoring of active ingredients in the calcium zinc gluconate oral solution, the active ingredients comprising calcium gluconate, zinc gluconate and/or lysine hydrochloride.

Description

HPLC-ELCD method for simultaneously detecting calcium gluconate, zinc gluconate and lysine hydrochloride and application thereof Technical Field The invention relates to the technical field of substance detection, in particular to an HPLC-ELCD method for simultaneously detecting calcium gluconate, zinc gluconate and lysine hydrochloride and application thereof. Background The calcium zinc gluconate oral solution can be used for treating problems caused by calcium deficiency and zinc deficiency, such as osteoporosis, tetany, bone hypoplasia, rickets, calcium supplement for pregnant women, lactating women, menopausal women, infantile growth and development retardation, anorexia, recurrent oral ulcer, acne, etc. The calcium zinc gluconate oral solution is a compound preparation, and the active ingredients comprise calcium gluconate, zinc gluconate and lysine hydrochloride, and the current detection scheme can only independently detect the calcium gluconate, the zinc gluconate or the lysine hydrochloride. The method for measuring the calcium gluconate and the zinc gluconate comprises a titration method, an ion chromatography method, a method for measuring the lysine hydrochloride comprises a nitrogen determination method, a high performance liquid chromatography-evaporative light scattering detection method and an ion chromatography method, wherein the end point of the titration method is not easy to judge, the error is large, the experiment time of the nitrogen determination method is too long and at least needs 2 hours to complete, the sensitivity of the high performance liquid chromatography-evaporative light scattering detection method is relatively low, a mobile phase is required to be volatile and a non-volatile buffer salt and a surfactant cannot be used, the ion chromatography equipment is relatively expensive, and the development cost is relatively high. In order to realize the efficient detection of all main components of the calcium zinc gluconate oral solution, further research on a detection method is necessary. Disclosure of Invention The invention aims to provide an ideal method for simultaneously detecting calcium gluconate, zinc gluconate and lysine hydrochloride. The invention provides an HPLC-ELCD method for simultaneously detecting calcium gluconate, zinc gluconate and lysine hydrochloride, which adopts a cation exchange chromatographic column to carry out isocratic elution of a sample to be detected, wherein a mobile phase is a methylsulfonic acid-oxalic acid solution, the concentration of methylsulfonic acid in the methylsulfonic acid-oxalic acid solution is 0.002mol/L-0.004mol/L, and the concentration of oxalic acid is 0.12g/L-0.18g/L. According to the research of the invention, when the sample containing calcium gluconate, zinc gluconate and lysine hydrochloride is detected, the three substances can be effectively separated by adopting a high performance liquid chromatography combined with a conventional conductivity detector (ELCD) and using a cation exchange chromatographic column under a specific mobile phase, so that the simultaneous detection of the calcium gluconate, the zinc gluconate and the lysine hydrochloride is realized. The conditions of three substances can be quantitatively/qualitatively judged at the same time by carrying out one-time detection on the sample to be detected without designing chromatographic detection conditions for each substance, so that the time and cost of sample analysis are greatly shortened. Preferably, the concentration of methylsulfonic acid in the mobile phase of the HPLC-ELCD method of the present invention is 0.003mol/L and the concentration of oxalic acid is 0.15g/L. In the HPLC-ELCD method of the present invention, the chromatography column is Dionex IonPac TM SCS A. In the HPLC-ELCD method, the column temperature is 30+/-5 ℃, the flow rate is 1+/-0.2 ml/min, and the sample injection amount is 5-25 μl. The method adopts a conventional high performance liquid chromatography column and is provided with a conductivity detector, so that the detection is convenient and accurate compared with the traditional titration method or high performance liquid chromatography detection method, and the detection equipment has low price and stronger operability compared with ion chromatography. The invention also provides application of the HPLC-ELCD method in detecting calcium zinc gluconate oral solution. The invention also provides a method for simultaneously detecting calcium gluconate, zinc gluconate and lysine hydrochloride in the calcium zinc gluconate oral solution, which is used for detecting the calcium zinc gluconate oral solution sample by the HPLC-ELCD method. In the method of the invention, the sample is diluted with water prior to detection. In the method of the present invention, the method further comprises the step of quantifying calcium gluconate, zinc gluconate and/or lysine hydrochloride by an external standard method after detecting calciu