Methods and Objects of Chemical Analysis最新文献

Systematic Review and Guidelines for Management of Scrotal Inguinal Hernias. 阴囊腹股沟疝管理的系统性回顾和指南。

Q4 CHEMISTRY, ANALYTICAL

Methods and Objects of Chemical Analysis

Pub Date : 2023-03-27 eCollection Date: 2023-01-01 DOI: 10.3389/jaws.2023.11195

Hanh Minh Tran, Ian MacQueen, David Chen, Maarten Simons

Introduction: Of the more than 20 million patients undergoing groin hernia repair annually worldwide, 6% are scrotal hernias in high resource countries rising to 67% in low resource countries which represents a heavy disease burden on relatively young men during their most productive period of life. There are many open questions concerning management of scrotal hernia. These guidelines aim to improve the care for scrotal hernia patients by reducing recurrence rates, chronic pain and infection. Methods: After developing 19 key questions a systematic literature review was performed till 31 March 2021 for all relevant publications with search terms related to Scrotal Hernia. The articles were scored by all co-authors according to Oxford, SIGN and Grade methodologies. Statements and recommendations were formulated. Online Consensus meetings with 25 HerniaSurge members were organised with voting and grading Recommendations as "strong" (recommendations) or "weak" (suggestions) and by consensus, in some cases upgraded. Results: Only 23 articles (two level 2 registry and 21 level 3-5) were selected. It is proposed to define scrotal hernia as an inguinal hernia which has descended into and causes any scrotal distortion. A new classification for scrotal hernias was proposed based on hernia size, SI for upper third thigh, SII for middle thigh and SIII for lower third thigh or below. Irreducibility is denoted with IR. Despite weak evidence antibiotic prophylaxis is recommended. Urinary catheterization is recommended (upgraded) in complex cases (S2-3) due to prolonged operative time. Scrotal hernia repairs have higher associated morbidity and mortality compared to non-complex groin hernia repairs irrespective of surgical experience. Open anterior (mesh) approach is commonest technique and suture techniques in low resource countries. For minimally invasive approaches, TAPP resulted in less conversion to open approach compared to TEP. Conclusion: Although the evidence is scarce and often low quality scrotal hernia management guidelines aim to lead to better surgical outcomes irrespective of where patients live. This necessarily means a more tailored approach based on available resources and appropriate skills. The guidelines provide an impetus for future research where adoption of proposed classification will enable more meaningful comparison of different techniques for different hernia sizes.

导言：在全球每年接受腹股沟疝修补术的 2000 多万名患者中，资源丰富国家的阴囊疝患者占 6%，而资源匮乏国家的比例则高达 67%，这意味着相对年轻的男性在其一生中最有生产力的时期承受着沉重的疾病负担。关于阴囊疝的治疗，还有许多问题尚未解决。本指南旨在通过减少复发率、慢性疼痛和感染来改善阴囊疝患者的治疗。方法：提出 19 个关键问题后，在 2021 年 3 月 31 日前对所有与阴囊疝相关的出版物进行了系统性文献回顾。所有共同作者根据牛津、SIGN 和等级方法对文章进行评分。制定了声明和建议。由 25 名疝气研究小组成员参加的在线共识会议组织了投票，并将建议分为 "强"（建议）或 "弱"（建议）等级，在某些情况下，通过共识将建议升级。结果：只有 23 篇文章（2 篇 2 级登记文章和 21 篇 3-5 级文章）入选。建议将阴囊疝定义为腹股沟斜疝并导致阴囊变形。根据疝气的大小，提出了阴囊疝的新分类方法：SI 表示大腿第三上段，SII 表示大腿中部，SIII 表示大腿第三下段或以下。不可还原性用 IR 表示。尽管证据不足，但仍建议使用抗生素预防。由于手术时间较长，建议在复杂病例（S2-3）中使用导尿管（升级版）。与非复杂的腹股沟疝修补术相比，无论手术经验如何，阴囊疝修补术的相关发病率和死亡率都较高。在资源匮乏的国家，开放式前部（网状）方法是最常见的技术，也是最常用的缝合技术。就微创方法而言，TAPP 与 TEP 相比，转为开放式方法的情况较少。结论：尽管证据稀少，而且往往质量不高，但阴囊疝管理指南的目标是，无论患者居住在哪里，都能获得更好的手术效果。这必然意味着要根据可用资源和适当技能采取更有针对性的方法。该指南为未来的研究提供了动力，在未来的研究中，采用建议的分类方法将能对不同疝气大小的不同技术进行更有意义的比较。

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引用次数: 0

Development, Optimization, and Validation of a Novel HPLC Method for Simultaneous Quantification of Artesunate and Amodiaquine in Tablet Formulations 同时测定片剂中青蒿琥酯和阿莫地喹含量的高效液相色谱方法的建立、优化和验证

IF 0.7 Q4 CHEMISTRY, ANALYTICAL

Methods and Objects of Chemical Analysis

Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.42-50

Fouad Echerfaoui, H. Bouchafra, K. El Bourakadi, A. El Orche, Mounir El Kacemi, Abdelhafid Benomar, K. Karrouchi, M. Bouatia, M. El Karbane

Artemisinin-based combination therapy (ACTs) has become the primary first-line treatment for mild falciparum malaria in the majority of African countries. A fixed-dose combination of amodiaquine and artesunate is commonly employed to enhance treatment compliance and achieve successful malaria outcomes. In this study, a specific, accurate, linear, precise, and repeatable method was optimized, verified, and applied for the simultaneous estimation of artesunate and amodiaquine HCl in a commercially available artesunate-amodiaquine tablet with a dosage of 100 mg/270 mg. The optimization process involved two steps. Firstly, the top three were carefully selected out of seven characteristics influencing the separation. These key elements required fine-tuning, namely the column type, ion pair, and the residual amount of acetonitrile (ACN) remaining after elution. In the second step, a Box-Behnken experimental design, coupled with Derrenguer's desirability approach, was utilized to identify the ideal target conditions. The optimized method demonstrated excellent specificity, accuracy, linearity, precision, and repeatability, allowing for the reliable simultaneous estimation of artesunate and amodiaquine HCl in the artesunate-amodiaquine tablet. This method offers a valuable tool for quality control and dosage determination in the pharmaceutical industry. By employing advanced experimental techniques and focusing on critical parameters, the study contributes to analytical methodologies in malaria treatment.

在大多数非洲国家，以青蒿素为基础的联合疗法已成为治疗轻度恶性疟疾的主要一线疗法。通常采用阿莫地喹和青蒿琥酯的固定剂量组合来提高治疗依从性并取得成功的疟疾治疗结果。本研究对市售剂量为100mg / 270mg的青蒿琥酯-阿莫地喹片剂中盐酸阿莫地喹和青蒿琥酯含量的同时测定方法进行了优化、验证和验证。优化过程包括两个步骤。首先，从影响分离的7个特征中精心挑选出前3个特征。这些关键元素需要微调，即柱类型、离子对和洗脱后乙腈(ACN)的残留量。第二步，采用Box-Behnken实验设计，结合Derrenguer的可取性方法，确定理想的目标条件。优化后的方法具有良好的专属性、准确度、线性度、精密度和重复性，可可靠地同时测定青蒿琥酯-阿莫地喹片中盐酸阿莫地喹和青蒿琥酯的含量。该方法为制药行业的质量控制和剂量测定提供了有价值的工具。通过采用先进的实验技术和关注关键参数，该研究有助于疟疾治疗的分析方法。

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引用次数: 0

Study of the Biochemical Potential of Wild Fruit of the Caucasus Medar (Mespilus caucasics L.) in the Post-Harvest Period 高加索Medar (Mespilus caucasics L.)野生果实收获后生化势的研究

IF 0.7 Q4 CHEMISTRY, ANALYTICAL

Methods and Objects of Chemical Analysis

Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.29-32

É. B. Farzaliev

The carbohydrate complex (fructose, glucose, sucrose, pectin substances), the main organic and fatty acids, which are important food functional ingredients, were studied in the wild fruits of the Caucasian loquat during their storage. It has been established that during 40 days of storage there are significant changes in the biochemical potential of fruits for almost all the studied food ingredients, the level of their final content is 5-10 % of the original content.

对高加索枇杷野生果实在贮藏过程中的碳水化合物(果糖、葡萄糖、蔗糖、果胶物质)、主要有机酸和脂肪酸等重要食品功能成分进行了研究。研究表明，在贮藏40天内，几乎所有被研究的食品成分的生化势都发生了显著变化，其最终含量为原始含量的5- 10%。

引用次数: 0

Application of Enzymatic Photometric Kinetic Method for Determination of Benzalkonium Chloride in Various Dosage Forms 酶光度动力学法测定不同剂型苯扎氯铵的应用

IF 0.7 Q4 CHEMISTRY, ANALYTICAL

Methods and Objects of Chemical Analysis

Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.5-12

M. Blazheyevskіy, O. Koval’ska

A kinetic-photometric method for accurate and sensitive determination of benzalconium chloride has been described. The method is based on inhibition of enzymatic hydrolysis of acetylcholine by enzyme acethylcholinestherase reaction. The amount of benzalconium chloride was determined by the degree of inhibition of the enzymatic reaction, which was evaluated by the residual unreacted substrate - acetylcholine. Determination of the residual amount of acetylcholine in the reaction mixture was performed by a kineticphotometric method using an indicator oxidation reaction of p-phenetidine with peracetic acid, which is formed during the auxiliration reaction of perhydrolysis with addition of excess hydrogen peroxide in the reaction mixture over a period of time. The inhibition degree –concentration plot is linear over the range of 1.4 ∙10-6 – 7.0∙10-6 mol/ L with correlation coefficient of 0.998. The LOQ was 1.9∙10-6 mol/L. The different experimental parameters pH, buffer solution was carefully studied and optimized. The proposed method has been successfully applied to pharmaceutical formulations. Statistical comparison of the results with a good established reported method showed excellent agreement and proved that there is no significant difference in the accuracy and precision. For “Virotec-intim” preparation RSD was 3.2 % (δ*=- 0.3 %).

介绍了一种准确灵敏地测定苯扎氯铵的动力学光度法。该方法以乙酰胆碱酯酶反应抑制乙酰胆碱酶解为基础。通过酶促反应的抑制程度来确定苯扎氯铵的用量，并通过剩余未反应底物乙酰胆碱来评价其抑制程度。反应混合物中乙酰胆碱残留量的测定采用动力学光度法，利用对非尼替丁与过氧乙酸的指示剂氧化反应，该反应是在反应混合物中加入过量的过氧化氢一段时间的过水解辅助反应过程中形成的。抑制度-浓度曲线在1.4∙10-6 ~ 7.0∙10-6 mol/ L范围内呈线性关系，相关系数为0.998。LOQ为1.9∙10-6 mol/L。对不同的实验参数pH、缓冲液进行了仔细的研究和优化。所提出的方法已成功地应用于药物制剂。将结果与已建立的方法进行统计比较，结果非常一致，证明在准确度和精密度上没有显著差异。“Virotec-intim”制剂的RSD为3.2% (δ*=- 0.3%)。

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引用次数: 0

Analytical Validation of a Reversed-Phase Ion Pairing HPLC-DAD Method for the Simultaneous Determination of Anthropogenic Pollutants 反相离子配对HPLC-DAD法同时测定人为污染物的分析验证

IF 0.7 Q4 CHEMISTRY, ANALYTICAL

Methods and Objects of Chemical Analysis

Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.13-21

Liew Sook Ling, Ivan Kok Seng Yap, Chong Chun Wie, Wong Lai Chun

Caffeine, trigonelline, nicotinamide, and hippuric acid are potential organic markers of anthropogenic activities in the environment. In this work, a selective, precise, accurate, and robust reverse phase high performance liquid chromatography with a diode array detection method was developed for their simultaneous determination. Chromatographic analysis was achieved on GraceSmart RP C18 (150 mm x 4.6 mm, 5 μm) column. The mobile phase was 20 mM ammonium acetate buffer (pH 4.5) and methanol in gradient elution mode at a flow rate of 1.0 mL min-1, with 5 mM heptafluorobutyric acid as an ion pairing agent. Detection was performed at 275 nm for caffeine, 265 nm for trigonelline, 261 nm for nicotinamide, and 250 nm for hippuric acid. The method was validated as per the International Conference on Harmonization guidelines. Linear responses were found in the concentration range of 10-200 μg mL-1 with a correlation coefficient of at least 0.999. The percent relative standard deviation of intra-day precision, inter-day precision, and robustness was less than 2 %. The accuracy, expressed as percentage recovery ranged between 93.23 – 99.22%. Values for limits of detection and quantification were between 0.07-0.34 μg mL-1, and 0.21-1.04 μg mL-1, respectively. Lake samples from public parks were collected and subjected to analysis using the validated method

咖啡因、葫芦巴碱、烟酰胺和马尿酸是环境中人类活动的潜在有机标志物。本研究建立了一种选择性、精密度、准确度和鲁棒性强的反相高效液相色谱二极管阵列检测方法。色谱分析采用GraceSmart RP C18 (150 mm x 4.6 mm, 5 μm)色谱柱。流动相为20 mM醋酸铵缓冲液(pH为4.5)和甲醇，梯度洗脱，流速为1.0 mL min-1, 5 mM七氟丁酸为离子配对剂。咖啡因的检测波长为275 nm，葫芦巴碱为265 nm，烟酰胺为261 nm，马尿酸为250 nm。该方法按照国际协调会议的准则进行了验证。在10 ~ 200 μ mL-1浓度范围内呈线性关系，相关系数至少为0.999。日内精密度、日内精密度和稳健性的相对标准偏差百分比小于2%。准确度在93.23 ~ 99.22%之间，以回收率表示。检出限为0.07 ~ 0.34 μ mL-1，定量限为0.21 ~ 1.04 μ mL-1。采集公园湖泊样本，采用验证方法进行分析

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引用次数: 0

Chromatographic Determination of the Chemical Composition of Apple Chips Extract 苹果片提取物化学成分的色谱测定

IF 0.7 Q4 CHEMISTRY, ANALYTICAL

Methods and Objects of Chemical Analysis

Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.33-41

O. Hulai, V. Shemet, O.S. Klimovych

The qualitative composition of the extraction of dried apples of green (Golden, Mutsu) and red (Florina, Aidared) varieties by gas-liquid chromatography with mass-selective detection has been established. The chips were obtained by convective drying at the temperature of +(63–70) °С to a final dampness of 6–8 %. Water-alcohol extract was analyzed on the Shimadzu GCMS-QP2020 gas chromatomas-spectrometer with a full ion current (SCAN), the scanning range of 40–1000 Da. The peaks were processed and identified based on the open source data (NIST 2017 and Wiley 5th Edition). In the studied samples of apple extraction, 30 characteristic components were found, among which carbohydrates predominate – mono- and disaccharides, their derivatives and products of dehydration and oxidation. The apple extract contains higher fatty acids: n-hexadecanoic acid, tetradecanoic acid, octadecanoic acid, oleic acid. Compounds formed as a result of drying (5-hydroxymethylfurfural, 3,5-dihydroxy-6-methyl-2,3-dihydro-4H-pyrane-4-one), as well as flavonoids and anthocyanins, which perform antioxidant and weak antibiotic functions in the body, were identified. Vitamins could not be determined using this method.

建立了青苹果(Golden、Mutsu)和红苹果(Florina、aibold)干提取物的气液色谱质谱鉴别方法。薄片在+(63-70)°С温度下对流干燥，最终湿度为6 - 8%。水醇提取物在岛津GCMS-QP2020气相色谱仪上进行全离子电流(SCAN)分析，扫描范围为40-1000 Da。根据开源数据(NIST 2017和Wiley 5th Edition)对峰值进行处理和识别。在研究的苹果提取液样品中，发现了30种特征成分，其中以碳水化合物为主——单糖和双糖及其衍生物和脱水氧化产物。苹果提取物含有较高的脂肪酸:正十六酸、十四酸、十八酸、油酸。经干燥后形成的化合物(5-羟甲基糠醛，3,5-二羟基-6-甲基-2,3-二氢- 4h -pyrane-4-one)，以及黄酮类和花青素，在体内具有抗氧化和弱抗生素功能。维生素不能用这种方法测定。

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引用次数: 0

Simultaneous Quantitative Determination of Eight Fluoroquinolones by High-Performance Liquid Chromatography with UV Detection using a C18 Monolithic Column C18整体柱高效液相色谱-紫外检测同时定量测定8种氟喹诺酮类药物

Q4 CHEMISTRY, ANALYTICAL

Methods and Objects of Chemical Analysis

Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.101-108

Emna Toujani, Wafa Belgaied, Sana Toujani

In the present work, an accurate and reliable reversed-phase liquid chromatographic method (RP-HPLC) for the simultaneous quantitative determination of eight fluoroquinolones (enoxacin, norfloxacin, ciprofloxacin, levofloxacin, moxifloxacin, enrofloxacin, sparfloxacin, and marbofloxacin) in bulk form and in pharmaceutical products is described. The optimum separation of the selected pharmaceutical compounds was achieved on a Chromolith® RP-18 endcapped column with a mobile phase consisting of acetonitrile and phosphate buffer (pH 5.5; 15 mM) pumped at 2 mL min-1. UV detection of all compounds was accomplished at 280 nm. The procedure was validated according to the International Conference on Harmonization (ICH) Q2 (R1) guideline. Good linear relationships were obtained (r ≥ 0.996) for all the analytes over their respective concentration ranges. Intra- and inter-day precision were less than 2 %. Recoveries were held in the range of 98 to 102 %. The developed method was successfully applied to the analysis of pharmaceutical products.

本文建立了一种准确可靠的反相液相色谱法(RP-HPLC)，用于同时定量测定原料药和制剂中8种氟喹诺酮类药物(依诺沙星、诺氟沙星、环丙沙星、左氧氟沙星、莫西沙星、恩诺沙星、斯帕沙星和马布沙星)的含量。在所选药物化合物的最佳分离是在Chromolith®RP-18端盖柱上实现的，流动相为乙腈和磷酸盐缓冲液(pH 5.5;15mm)泵在2ml min-1。所有化合物的紫外检测均在280 nm完成。该程序根据国际协调会议(ICH) Q2 (R1)指南进行验证。各分析物在各自浓度范围内均具有良好的线性关系(r≥0.996)。日内和日内精度均小于2%。加样回收率在98% ~ 102%之间。该方法已成功地应用于药品的分析。

引用次数: 0

Partial Least Squares Method for the Multicomponent Analysis of Antibacterial Mixture 抗菌合剂多组分分析的偏最小二乘法

Q4 CHEMISTRY, ANALYTICAL

Methods and Objects of Chemical Analysis

Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.92-100

Farah Nouri, Nahla A. Alassaf

This study's objective is to assess how well UV spectrophotometry can be used in conjunction with multivariate calibration based on partial least squares (PLS) regression for concurrent quantitative analysis of antibacterial mixture (Levofloxacin (LIV), Metronidazole (MET), Rifampicin (RIF) and Sulfamethoxazole (SUL)) in their artificial mixtures and pharmaceutical formulations. The experimental calibration and validation matrixes were created using 42 and 39 samples, respectively. The concentration range taken into account was 0-17 μg/mL for all components. The calibration standards' absorbance measurements were made between 210 and 350 nm, with intervals of 0.2 nm. The associated parameters were examined in order to develop the optimal calibration model. The cross-validation method was used to determine the ideal number of components. The coefficient of determination (R2) and the root mean square error of calibration (RMSEC) are used to evaluate the calibration model. The relation between the LEV, MET, RIF, and SUL actual values and predicted values had a coefficient of determination that was higher than 0.997, showing very good accuracy of the devised approach. The obtained RMSEC values, 0.181056465 (LEV), 0.180375418 (MET), 0.142767171 (RIF), and 0.17157454 (SUL), show an analytical procedure with adequate precision. The suggested technique for quantitative analysis of the quaternary mixture of LEV, MET, RIF, and SUL have been applied successfully in different pharmaceutical preparations. The UV spectrophotometry assisted with chemometric-PLS without prior treatment, be utilised to resolve multicomponent mixtures successfully.

本研究的目的是评估紫外分光光度法与基于偏最小二乘(PLS)回归的多变量校准相结合，在抗菌药物混合制剂(左氧氟沙星(LIV)、甲硝唑(MET)、利福平(RIF)和磺胺甲恶唑(SUL))的人工混合物和药物制剂中同时定量分析的效果。分别用42个和39个样品建立了实验校准矩阵和验证矩阵。所考虑的浓度范围为0 ~ 17 μg/mL。校准标准品的吸光度测量在210 ~ 350 nm之间，间隔为0.2 nm。为了建立最优的标定模型，对相关参数进行了检验。采用交叉验证法确定理想组分数。采用决定系数(R2)和标定均方根误差(RMSEC)对标定模型进行评价。LEV、MET、RIF、SUL的实际值与预测值之间的决定系数均大于0.997，表明所设计的方法具有很好的准确性。获得的RMSEC值为0.181056465 (LEV)， 0.180375418 (MET)， 0.142767171 (RIF)和0.17157454 (SUL)，显示了具有足够精度的分析过程。该方法已成功地应用于不同药物制剂的四元化合物中，包括LEV、MET、RIF和SUL。紫外分光光度法辅助化学计量- pls无需事先处理，成功地解决了多组分混合物。

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引用次数: 0

Extraction of Alkaloids by the Micellar Phase of Sodium Dodecyl Sulfate for their Further Chromatographic Determination 十二烷基硫酸钠胶束相萃取生物碱的进一步色谱测定

Q4 CHEMISTRY, ANALYTICAL

Methods and Objects of Chemical Analysis

Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.81-86

V.S. Starova, S.A. Kulichenko

The influence of the main parameters of hydrophobicity (log P), structure (PSA), and protolytic properties (pKa) of some alkaloids on their distribution into modified micellar extraction system based on sodium dodecyl sulfate (SDS-NaCl-H2Sal) was established. The proposed prognostic regression D= 941 – 4.09∙PSA – 27.3∙log P – 44.5∙рКа is characterized by satisfactory indexes (R-squared 99.9, F-ratio 242, standard error 7.19, mean absolute error 2.38). The accuracy of the alkaloid distribution prediction by this regression is well correlated with accuracy of the measurement of the extraction parameters. The predicted D value for novocaine is 257 (R = 93 %), and the experimentally found D value is 202 (R = 91 %). For lidocaine, the predicted and experimental D values are practically the same and equal 386 (R = 95 %) and 380 (R = 95 %), respectively. The possibility of quantitative extraction of positively charged hydrophilic (logP < 0) organic bases into the micellar phase of SDS is shown. The developed hybrid HPLC technique for determining papaverine in urine with its cationic form (pH=2) preconcentration by modified micellar SDS phase is characterized by sufficient sensitivity and accuracy (DL= 0.01 μg/ml, Sr ≤ 0.08, R > 99 %, K = 10). Only alkaloids with log P > 1.4 can be determined by this technique because otherwise, the chromatographic peaks of salicylic acid and alkaloid cannot separate.

研究了部分生物碱的疏水性(log P)、结构(PSA)和水解性能(pKa)等主要参数对其在十二烷基硫酸钠(SDS-NaCl-H2Sal)改性胶束萃取体系中的分布的影响。所提出的预后回归D= 941 - 4.09∙PSA - 27.3∙log P - 44.5∙рКа指标令人满意(r方99.9,f比242，标准误差7.19，平均绝对误差2.38)。该回归预测生物碱分布的准确度与提取参数测量的准确度具有良好的相关性。对诺佛卡因的预测D值为257 (R = 93%)，实验发现D值为202 (R = 91%)。利多卡因的预测D值与实验D值基本一致，分别为386 (R = 95%)和380 (R = 95%)。带正电的亲水性(logP <0)有机碱进入SDS胶束相。采用改性胶束SDS相对尿液中阳离子形态(pH=2)的罂粟碱进行预富集的混合高效液相色谱技术具有足够的灵敏度和准确性(DL= 0.01 μg/ml, Sr≤0.08,R >99%， k = 10)。只有生物碱具有对数P >1.4由于水杨酸和生物碱的色谱峰不能分离，所以可以用该技术进行测定。

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引用次数: 0

Determination of Mycotoxins in Wheat Grain by LC-MS/MS using Modified QuEChERS Sample Preparation 改良QuEChERS样品制备的LC-MS/MS法测定小麦籽粒中的真菌毒素

IF 0.7 Q4 CHEMISTRY, ANALYTICAL

Methods and Objects of Chemical Analysis

Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.22-28

S. Senin, S. Midyk, V. Korniyenko, O. Konovalova, O. V. Berezovskyi, E. Ladohubets, I. Harkusha

The procedure of the mycotoxins determination in wheat grain was developed by LC-MS/MS using modified QuEChERS sample preparation. The method of simultaneous determination of six mycotoxins (aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, T-2 toxin and zearalenone) in wheat grain was validated according to the following criteria: specificity, linearity, limits of detection (LOD), limits of quantification (LOQ), accuracy, and precision. The chromatographic and mass spectrometric conditions for separation and determination of the mycotoxins were optimized during the study. It was established that the most optimal mobile phase for the separation of six mycotoxins is 5 mМ ammonium formate solution in methanol : water : formic acid (5 : 94.9 : 0.1 by volume, eluent A and 95:4.9:0.1 by volume, eluent B). It was found that the correlation coefficients for six mycotoxins range from 0.9990 to 0.9998 (R2 > 0.995). Limits of detection (LOD) and limits of quantification (LOQ) of the mycotoxins are below the maximum permitted levels set by the European Union (EU). Percent recovery in the range from 88 to 103 % indicates the acceptability of the mycotoxin extraction procedure. The relative standard deviation (RSD, %) of the measurement results under conditions of repeatability ranged from 1.94 to 8.76 %. The obtained data suitability evaluation of method (validation) corresponds to criteria European Commission Regulation (EC) No. 401/2006. The validation results showed that LC-MS/MS method with using of modified QuEChERS sample preparation is effective and suitable for the simultaneous quantitation of mycotoxins in wheat grain.

采用改良的QuEChERS样品制备技术，建立了小麦中真菌毒素的LC-MS/MS检测方法。根据特异性、线性度、检出限(LOD)、定量限(LOQ)、准确度、精密度等标准，建立了同时测定小麦籽粒中黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、T-2毒素和玉米赤霉烯酮6种真菌毒素的方法。优化了真菌毒素分离测定的色谱和质谱条件。结果表明，分离6种真菌毒素的最佳流动相为5 mМ甲酸铵溶液(5∶94.9∶0.1体积(洗脱液A)和95∶4.9∶0.1体积(洗脱液B))， 6种真菌毒素的相关系数为0.9990 ~ 0.9998 (R2 > 0.995)。真菌毒素的检出限(LOD)和定量限(LOQ)低于欧洲联盟(EU)规定的最大允许水平。回收率在88%至103%范围内表明霉菌毒素提取程序的可接受性。在重复性条件下，测定结果的相对标准偏差(RSD， %)范围为1.94 ~ 8.76%。获得的数据适用性评估方法(验证)符合欧盟委员会法规(EC) No 401/2006的标准。验证结果表明，采用改良的QuEChERS样品制备的LC-MS/MS方法是有效的，适用于小麦籽粒中真菌毒素的同时定量。

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引用次数: 0