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A method for detecting nitrosamine impurities in biapenem

A technology of nitrosamines and detection methods, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problem of high detection sensitivity and achieve the effects of reducing influence, reducing matrix effect, and avoiding inhibition

Active Publication Date: 2021-12-28
广州国标检验检测有限公司
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the detection methods of nitrosamine impurities are mainly gas chromatographic thermal analysis, spectrophotometry, gas-mass method and liquid-mass method. The detection method of nitrosodiisopropylamine
At the same time, the limit of nitrosamine impurities in biapenem (0.022ppm) is extremely low, and the requirements for detection sensitivity are high. It is difficult for existing detection methods to achieve the quantitative monitoring of nitrosamine impurities in biapenem

Method used

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  • A method for detecting nitrosamine impurities in biapenem
  • A method for detecting nitrosamine impurities in biapenem
  • A method for detecting nitrosamine impurities in biapenem

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Experimental program
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Embodiment 1

[0042] 1. Liquid chromatography conditions: Chromatographic column: Waters ACQUITY UPLC HSS T3 column (1.8μm, 2.1mm×100mm); mobile phase A: 0.1% formic acid-water, mobile phase B: methanol; column temperature 40 ℃; flow rate 0.3ml / min;

[0043] The elution program is: 0~3min, A 95%, B 5%; 3.5~4.5min, A 90%, B 10%; 5.5~6.5min, A60%, B40%; 7~8min, A 20%, B 80%; 8.1~9.5min, A 0%, B 100%; 9.6~12min, A 95%, B 5%.

[0044] 2. Mass spectrometry conditions: ion source APCI source, scan mode MRM, ion pair: N-nitrosoethylisopropylamine (EIPNA) 117.1 / 75.1, collision energy 15V; N-nitrosodiisopropylamine (DIPNA) 131.1 / 89.1, collision energy 15V; N-nitrosodiethylamine (NDEA) 103.1 / 47.0, collision energy 29V; internal standard NDEA-d4 107.0 / 77.0, collision energy 16V; internal standard NDPA-d14 145.0 / 50.0, collision Can be 19V.

[0045] 3. Mixed solvent preparation: Take 20ml of methanol and put it in a reagent bottle, add 170ml of water, then add 10ml of formic acid, and shake well. ...

Embodiment 2

[0052] With reference to the detection method of embodiment 1, detection result is as follows:

[0053] 1. Exclusiveness

[0054] The reference substance solution and the spiked solution with a concentration of 1.319 ng / ml were taken respectively for sample testing, and the recorded chromatograms are shown in Figure 1~6 shown. The figure shows that the peak position of the target peak in the 100% limit concentration spiked test solution has no interference from other impurities, and is similar to the peak shape of the 100% limit concentration reference solution, indicating that the detection method has good specificity.

[0055] 2. Linear

[0056] The standard curve solution was taken for sample loading test, and the linear fitting equation was obtained through the relationship between peak area and concentration, as shown in Table 1 below. For each impurity in each concentration range, the peak area ratio has a good linear relationship with the concentration, and the correl...

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Abstract

This application belongs to the technical field of drug analysis. The application provides a method for detecting nitrosamine impurities in biapenem, comprising: taking the test product and adding an internal standard methanol solution to dissolve, then adding a mixed solvent and mixing evenly to obtain a sample solution; mixing the sample solution and The reference substance solution was respectively injected into a liquid chromatography tandem mass spectrometer, and the content of nitrosamine impurities was detected by the internal standard method; wherein, the composition of the mixed solvent included methanol, formic acid and water. This application develops the method according to the characteristics of nitrosamine compounds, which can effectively reduce the influence of the matrix effect and prevent the analyte from being inhibited. The detection method of this application was verified from the aspects of specificity, linearity and range, detection limit, quantitation limit, accuracy, and stability, and confirmed that the method is suitable for the simultaneous determination of the contents of NDEA, EIPNA, and DIPNA in biapenem.

Description

technical field [0001] The application belongs to the technical field of drug analysis, and in particular relates to a method for detecting nitrosamine impurities in biapenem. Background technique [0002] Biapenem is a synthetic carbapenem antibiotic that produces nitrosamine by-products during the production process, such as N-nitrosodiethylamine, N-nitrosoethylisopropylamine and N- Nitrosodiisopropylamine. Nitrosamines are strong carcinogens, not only can cause cancer in animals or humans in a small dose for a long time, but also can cause cancer with a "shock" of a higher dose. [0003] At present, the detection methods of nitrosamine impurities are mainly gas chromatographic thermal analysis, spectrophotometry, gas-mass method and liquid-mass method. The detection method of nitrosodiisopropylamine. At the same time, the limit of nitrosamine impurities in biapenem (0.022ppm) is extremely low, and the requirements for detection sensitivity are high. It is difficult for...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/72G01N30/8675G01N2030/324
Inventor 陈新国邱全玉邵广志黄军建陈亿展曹丹麦华凤蒋杰
Owner 广州国标检验检测有限公司
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