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Quick central-control detection method for etimicin sulfate

A technology of etimicin and a detection method, applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve the problems of complex and uncontrollable derivatization reaction, influence of derivatization products, and influence on production efficiency of etimicin sulfate, etc. The effect of short detection time, high sensitivity and wide linear range

Active Publication Date: 2014-04-16
WUXI JIYU SHANHE PHARM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the control detection method in the production process of etimicin sulfate is pre-column derivatization high-performance liquid chromatography. Due to the complexity and uncontrollability of the derivatization reaction, the instability of the derivatization product affects the accuracy of the measurement results, and the detection time must be at least More than half an hour seriously affected the production efficiency of etimicin sulfate

Method used

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  • Quick central-control detection method for etimicin sulfate
  • Quick central-control detection method for etimicin sulfate
  • Quick central-control detection method for etimicin sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Experimental equipment and reagents:

[0034] 1. Experimental equipment:

[0035] Agilent 1260 infinity series, Waters acquity H-class UPLC

[0036] 2. Experimental reagents:

[0037] Etimicin sulfate intermediate product desorption solution (Wuxi Jimin Credible Shanhe Pharmaceutical Co., Ltd.), etimicin reference substance (China National Inspection Institute), methanol (chromatographically pure, Merck), acetonitrile (chromatographically pure, Merck), ammonia water (analytical pure, Chinese medicine), glacial acetic acid (analytical pure, Chinese medicine), ammonium acetate (analytical pure, Chinese medicine), ultrapure water (self-made).

[0038] 3. Chromatographic conditions:

[0039] Chromatographic column: the filler is octadecylsilane bonded silica gel, the particle size is 1.7~3.5μm, the column size is 50mm~150mm×1.0~4.6mm, and the column pore diameter is Mobile phase: divided into organic phase and aqueous phase, the organic phase is methanol or acetonitril...

Embodiment 2

[0074] 2.1 Chromatographic conditions

[0075] Chromatographic instrument: Agilent 1260 infinity series; Chromatographic column: Phenomenex Kinetex-C18 (50×4.6mm, 2.1μm); Mobile phase A: methanol, mobile phase B: water-ammonia-glacial acetic acid (98:2.0:1.0), according to Gradient elution was carried out in the table below.

[0076] Table 2-1 Gradient elution program

[0077] time (min)

Phase B ratio (%)

[0078] 0

20

1

25

4

25

6

60

8

60

9

90

10

90

11

20

[0079] Flow rate: 0.5ml / min; injection volume 10μl; drift tube temperature of evaporative light scattering detector is 55°C, nitrogen flow rate is 2.0L / min, Gain value is 1.

[0080] 2.2 Specificity

[0081] Pass the etimicin intermediate product containing ethanol through a 0.45 μm membrane, and inject the sample according to the above conditions. Etimicin and its related...

Embodiment 3

[0104] 3.1 Chromatographic conditions

[0105] Chromatographic instrument: Waters Acquity UPLC; Chromatographic column: Waters XBridge C18 (100×3.5mm, 1.7μm); Mobile phase A: methanol, mobile phase B: water-ammonia-glacial acetic acid (90:4.8:0.2), according to the table below Gradient elution was carried out.

[0106] Table 3-1 Gradient elution program

[0107] time (min)

Phase B ratio (%)

0

25

1

30

4

30

5

60

8

60

9

90

[0108] 10

25

[0109] Flow rate: 2ml / min; injection volume 1μl; drift tube temperature of evaporative light scattering detector is 70°C, nitrogen flow rate is 3.0L / min, Gain value is 5.

[0110] 3.2 Specificity

[0111] Pass the etimicin intermediate product containing ethanol through a 0.45 μm membrane, and inject the sample according to the above conditions. Etimicin and its related impurities were separated by baseline, and the chromatog...

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Abstract

The invention relates to a quick central-control detection method for etimicin sulfate, wherein UPLC (Ultra Performance Liquid Chromatography) or UHPLC-ELSD (Ultra High Pressure Liquid Chromatography-Evaporative Light Scattering Detector) is employed, and separated and purified etimicin sulfate stripping liquid containing ethanol is taken as a sample and directly subjected to analysis, thereby controlling the production process. The method provided by the invention employs the technology of combining the ultra performance liquid chromatography with evaporative light scattering, and thereby is capable of realizing online quick detection in the production process; and therefore, the purpose of indicating flow component collection and detection in the separation and purification processes is achieved. Besides, the method is convenient, quick, accurate and reliable.

Description

technical field [0001] The invention relates to a rapid detection method for the intermediate control of the production process of etimicin sulfate, in particular to a rapid detection method for the rapid determination of etimycin sulfate by combining a liquid chromatography instrument with a pressure resistance of not less than 600 bar and an evaporative light detector The intermediate product in the production process of etimicin sulfate achieves the purpose of controlling the production process of etimicin sulfate. Background technique [0002] Ultra-high performance liquid chromatography (UPLC) technology is a new chromatographic separation technology emerging with the introduction of Acquity UPLC, a chromatographic instrument operating under high pressure with small particle fillers, launched by Waters in 2003. Compared with high-performance liquid chromatography (HPLC) technology, it has the advantages of higher column efficiency and faster separation speed, so that an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 杨春艳邹济高石杰陆丹
Owner WUXI JIYU SHANHE PHARM CO LTD
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