Liquid chromatography tandem mass spectrometry (LC-MS/MS) method for detecting busulfan in plasma

A technology of liquid chromatography and tandem mass spectrometry, which is applied in the field of detection of busulfan in plasma by liquid chromatography and tandem mass spectrometry, which can solve the problems of long instrument analysis time, long method processing time, and insufficient analysis sensitivity, so as to save detection time , high precision, and shortened analysis time

Inactive Publication Date: 2020-02-04
上海药明傲喆医学检验所有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the current busulfan detection methods have their own shortcomings. For example, some analytical sensitivity is not enough, the lower limit of quantification is higher, and the upper limit is lower. Long; some instruments take a long time to analyze and use a large amount of samples

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  • Liquid chromatography tandem mass spectrometry (LC-MS/MS) method for detecting busulfan in plasma
  • Liquid chromatography tandem mass spectrometry (LC-MS/MS) method for detecting busulfan in plasma
  • Liquid chromatography tandem mass spectrometry (LC-MS/MS) method for detecting busulfan in plasma

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment one: specific implementation steps of the present invention

[0044] 1. Preparation of standard / quality control primary stock solution

[0045] 1.1 Standard primary stock solution (SSC): Busulfan standard methanol solution (Cerilliant) with a concentration of 1mg / mL, numbered as SSC, stored at -25~-15°C until the expiration date of the manufacturer;

[0046] 1.2 Quality control primary stock solution (SSQC): Weigh 10 mg of busulfan (TRC / Sigma) quality control with a million-level analytical balance, transfer to a 10 mL volumetric flask, and dilute to 10 mL with pure methanol to prepare The primary stock solution of the quality control product with a concentration of 1 mg / mL was shaken, mixed and ultrasonically transferred to a brown glass vial, numbered SSQC, and stored at -25 to -15°C with a validity period of one year.

[0047] 2. Preparation of secondary stock solution for standard / quality control

[0048] 2.1 Standard secondary stock solution (sub-SSC...

Embodiment 2

[0094] Example 2: Methodological verification

[0095] 1. Precision

[0096] Add corresponding amount of busulfan standard substance to blank matrix (100% bovine plasma heparin sodium anticoagulant), and prepare three concentration levels of busulfan in the linear range (25-7500ng / mL) of the calibration curve. The concentrations of Xiaoan standard solution are: 300ng / mL, 2500ng / mL, and 5000ng / mL. There are 3 parallel samples for each concentration level, which is a batch; a total of five batches are divided into 5 days for verification. a batch.

[0097] Table 5 precision data results

[0098] Busulfan Low concentration medium concentration High concentration Intra-assay precision (CV,%) 5.01 2.37 1.20 Inter-assay precision (CV,%) 3.43 3.79 3.04

[0099] The verification results are shown in Table 5. The CV% of the intra-assay and inter-assay precision is within 15%, which meets the verification requirements; and the CV% of the intra-as...

Embodiment 3

[0144] Example 3: Patient sample monitoring case

[0145] Case 1:

[0146] Basic information: Male, aged 47 years, weighing 75kg, administered intravenous dose of busulfan 120mg, completed venous blood collection 2 hours after intravenous drug injection, and 1, 4, 6, 8 hours after the first blood collection respectively Venous blood was collected, and the plasma was centrifuged as soon as possible and anticoagulated with sodium heparin. After performing sample pretreatment on the machine for sample analysis, a drug-time curve is established, such as Figure 6 shown.

[0147] Case 2:

[0148] Basic information: female, age 32, body weight 67.2kg, intravenous dose of busulfan 108mg, venous blood collection completed 2 hours after intravenous drug injection, and 1, 4, 6, 8 days after the first blood collection respectively Venous blood was collected every hour, and the plasma was centrifuged as soon as possible and added heparin sodium for anticoagulation. After performing...

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Abstract

The invention provides a liquid chromatography tandem mass spectrometry (LC- MS / MS) method for detecting busulfan in plasma. The method comprises the following steps: preparing a working solution; performing pretreatment; performing LC-MS / MS analysis; extracting a chromatogram, and fitting a calibration curve; and establishing a drug time curve graph. The LC-MS / MS method provided by the inventionoptimizes the method for detecting busulfan in human plasma, so that the analysis time is shortened to 2 minutes, and the analysis accuracy and precision and the data stability are ensured; and moreover, the method is simple in pretreatment process, short in time and easy to operate. The detection time is saved, the detection accuracy and reliability are ensured, and more accurate, stable, and high-precision and high-sensitivity detection data can be provided within shorter time.

Description

technical field [0001] The invention belongs to the technical field of therapeutic drug monitoring and pharmacokinetic analysis, and in particular relates to a method for detecting busulfan in blood plasma by means of liquid chromatography tandem mass spectrometry. Background technique [0002] Busulfan is an alkylating agent, which belongs to bifunctional alkylating agent of bismethylsulfonate, and is a non-specific drug for cell cycle, which can be used to ablate bone marrow cells before hematopoietic stem cell transplantation. After busulfan enters the human body, the ring structure of its sulfonate group opens, and it destroys the structure and function of DNA by alkylating with guanine in cellular DNA. [0003] Busulfan is usually administered intravenously at a dose of 0.8 mg / kg every 6 hours for 4 days, for a total of 16 doses. However, repeated administration of busulfan can gradually accumulate in the body, and excessive doses will lead to hepatic veno-occlusive di...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/04G01N30/06G01N30/34G01N30/72G01N30/86G01N30/32G01N30/30G01N30/88
CPCG01N30/02G01N30/04G01N30/06G01N30/34G01N30/72G01N30/8634G01N30/32G01N30/30G01N30/88G01N2030/045G01N2030/324G01N2030/8822
Inventor 朱月红王金文吴亦宵
Owner 上海药明傲喆医学检验所有限公司
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