scholarly journals Validation of the Method for Determination of Melamine and Investigation its Trace in Milk from Vietnam by LC-MS/MS

Author(s):  
Quang Hieu-Tran

This work describes a rapid, selective, and sensitive method by using liquid chromatography-tandem mass spectrometry (LC-MS/MS) to detect melamine (MEL) in milk and dairy products. The optimal conditions of liquid chromatographic separation extraction and mass spectroscopy of MEL have also been examined. The linear range for analyte detected by the method was 0.5÷100.0 ng/mL, with correlation coefficients was 0.999.  Mean recoveries of the method in the real samples at three spike levels (low, medium, and high) were within the range of 98.5% ÷102.5% (n =7). LOD, LOQ values of the method were 10 and 30 ng/mL, respectively. The influence of the matrix effect on the accuracy, repeatability, and recovery of the process was insignificant. The proposed method was used to quantify the content of this compound in various real samples, which were collected in Ho Chi Minh City-Vietnam in 2020.

1985 ◽  
Vol 68 (4) ◽  
pp. 693-696 ◽  
Author(s):  
Samy H Ashoor ◽  
Michael J Knox ◽  
Jacquelyn R Olsen, ◽  
Dru Ann Deger

Abstract Reported here is a simple liquid chromatographic (LC) method for the i determination of riboflavin in milk (liquid, evaporated, and dry), yogurt, ' and cheese. The method involves passing liquid samples or filtrates of semisolid and solid samples through a Clg cartridge. Retained riboflavin is then eluted with an aliquot of 50% methanol in 0.02M acetate buffer of pH 4. A volume of the eluate is injected into the LC system | consisting of a CJ8 column, a solvent of water-methanol-acetic acid (65 + 35 + 0.1, v/v) with a flow rate of 1 mL/min, and a UV detector set at 270 nm. The method is precise and accurate and compares i favorably with the present AOAC method. Moreover, it involves fewer sample preparation steps and has a total analysis time of less than 1 h.


2020 ◽  
Vol 2020 ◽  
pp. 1-9
Author(s):  
Quang Hieu Tran ◽  
Thanh Tan Nguyen ◽  
Kim Phuong Pham

A selective, sensitive, and rapid method by using ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the determination of histamine in fish and fish sauce was developed. The optimal conditions of liquid chromatographic separation and mass spectroscopy of histamine have also been investigated. The linear ranges of the method were 20.0 ÷ 1000 ng/mL, and the corresponding correlation coefficient was 0.9993. Mean recoveries of the analyte at three spike levels (low, medium, and high) were within the range of 98.5% ÷ 102.5% (n = 7). The limit of detection (LOD) and limit of quantification (LOQ) values were 3.83 and 11.50 ng/mL for the fish sauce sample and 4.71 and 14.12 ng/mL for the fish sample, respectively. The influence of the matrix effect on the accuracy, repeatability, and recovery of the method was negligible. The recommended method was applied to determine the content of this substance in 21 fish sauce samples and 4 kinds of fish samples, which were collected from Ho Chi Minh City, Vietnam, in 2019.


Molecules ◽  
2021 ◽  
Vol 26 (14) ◽  
pp. 4357
Author(s):  
Waritda Pookmanee ◽  
Siriwan Thongthip ◽  
Jeeranut Tankanitlert ◽  
Mathirut Mungthin ◽  
Chonlaphat Sukasem ◽  
...  

The method for the determination of primaquine (PQ) and 5,6-orthoquinone primaquine (5,6-PQ), the representative marker for PQ active metabolites, via CYP2D6 in human plasma and urine has been validated. All samples were extracted using acetonitrile for protein precipitation and analyzed using the ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) system. Chromatography separation was carried out using a Hypersil GOLDTM aQ C18 column (100 × 2.1 mm, particle size 1.9 μm) with a C18 guard column (4 × 3 mm) flowed with an isocratic mode of methanol, water, and acetonitrile in an optimal ratio at 0.4 mL/min. The retention times of 5,6-PQ and PQ in plasma and urine were 0.8 and 1.6 min, respectively. The method was validated according to the guideline. The linearity of the analytes was in the range of 25–1500 ng/mL. The matrix effect of PQ and 5,6-PQ ranged from 100% to 116% and from 87% to 104% for plasma, and from 87% to 89% and from 86% to 87% for urine, respectively. The recovery of PQ and 5,6-PQ ranged from 78% to 95% and form 80% to 98% for plasma, and from 102% to from 112% to 97% to 109% for urine, respectively. The accuracy and precision of PQ and 5,6-PQ in plasma and urine were within the acceptance criteria. The samples should be kept in the freezer (−80 °C) and analyzed within 7 days due to the metabolite stability. This validated UHPLC-MS/MS method was beneficial for a pharmacokinetic study in subjects receiving PQ.


2018 ◽  
Vol 2018 ◽  
pp. 1-12 ◽  
Author(s):  
Haiyan Lei ◽  
Jianbo Guo ◽  
Zhuo Lv ◽  
Xiaohong Zhu ◽  
Xiaofeng Xue ◽  
...  

This study reports an analytical method for the determination of nitroimidazole and quinolones in honey using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A modified QuEChERS methodology was used to extract the analytes and determine veterinary drugs in honey by LC-MS/MS. The linear regression was excellent at the concentration levels of 1–100 ng/mL in the solution standard curve and the matrix standard curve. The recovery rates of nitroimidazole and quinolones were 4.4% to 59.1% and 9.8% to 46.2% with relative standard deviations (RSDs) below 5.2% and the recovery rates of nitroimidazole and quinolones by the matrix standard curve ranged from 82.0% to 117.8% and 79% to 115.9% with relative standard deviations (RSDs) lower than 6.3% in acacia and jujube honey. The acacia and jujube honeys have stronger matrix inhibition effect to nitroimidazole and quinolones residue; the matrix inhibition effect of jujube honey is stronger than acacia honey. The matrix standard curve can calibrate matrix effect effectively. In this study, the detection method of antibiotics in honey can be applied to the actual sample. The results demonstrated that the modified QuEChERS method combined with LC-MS/MS is a rapid, high, sensitive method for the analysis of nitroimidazoles and quinolones residues in honey.


2012 ◽  
Vol 70 (4) ◽  
pp. 296-302 ◽  
Author(s):  
Victor Abrahamsson ◽  
Signe Hoff ◽  
Nikoline J. Nielsen ◽  
Marianne N. Lund ◽  
Mogens L. Andersen

2003 ◽  
Vol 66 (8) ◽  
pp. 1439-1443 ◽  
Author(s):  
JEONG-HUN KANG ◽  
FUSAO KONDO

This study was conducted to develop a selective and sensitive method for the determination of bisphenol A (BPA) levels in milk and dairy products. A method based on solvent extraction with acetonitrile and solid-phase extraction (SPE) was developed for the analysis of BPA in milk, yogurt, cream, butter, pudding, condensed milk, and flavored milk, and a method using two SPE cartridges (OASIS HLB and Florisil cartridge) for skim milk was also developed. The developed methods showed good recovery levels (77 to 102%) together with low detection limits (1 μg/liter for milk, yogurt, pudding, condensed milk, flavored milk, and skim milk and 3 μg/liter for cream and butter). These methods are simple, sensitive, and suitable for the analysis of BPA in milk and dairy products. When 40 milk and dairy products were analyzed by the proposed methods, BPA was not identified in noncanned products, but its levels ranged from 21 to 43 μg/kg in canned products, levels that were 60- to 140-fold lower than the migration limits in the European Union and Japan.


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