液相色谱-串联质谱法测定烤烟中甲基嘧啶磷的残留量

建立了液相色谱-串联质谱(HPLC-MS/MS)测定烤烟中甲基嘧啶磷的残留分析方法。试样采用乙腈提取,经GCB和C₁₈净化剂净化后,用HPLC-MS/MS对甲基嘧啶磷进行定量分析。实验结果表明,甲基嘧啶磷在添加水平为0.03~3 mg/kg条件下的回收率为86.9%~92.5%,相对标准偏差为4.2%~11.5%。方法的定量限(LOQ)为0.03 mg/kg。本方法操作简单快速,准确度好,灵敏度高,适用于烤烟中甲基嘧啶磷残留量的检测。     

QuEChERS-高效液相色谱串联质谱法测定甜橙中哒螨灵和螺螨酯

[目的]建立了甜橙全果、果肉、果皮、果渣、橙汁和精油等6项基质中哒螨灵和螺螨酯的QuEChERS-高效液相色谱-串联质谱分析检测方法(HPLC-MS/MS)。[方法]甜橙样品经乙腈提取,PSA、GCB、MgSO4净化,高效液相色谱-串联质谱仪配备电喷雾正离子多反应监测(MRM),外标法定量。[结果]甜橙6种基质通过此分析检测方法,哒螨灵和螺螨酯在0.001~1.25 mg/L质量浓度范围线性相关系数不小于0.9965,3个加标水平(0.01、0.5、5 mg/kg)下哒螨灵回收率为81%~93%,RSD为0.5%~6.5%,螺螨酯回收率为81%~99%,RSD为0.5%~7.9%。[结论]该方法简单、方便、灵敏度、准确度高,覆盖甜橙全项样品基质,可适用于大批量样品快速分析。     

亚苄基海因水解制备苯丙酮酸过程的色-质联用分析

针对亚苄基海因水解体系建立了一种高效实用的液相色谱分析方法,为生产工艺控制提供了依据,并应用液-质联用技术对此体系中的未知副产物进行了初步检测。具体液相色谱条件为:流动相:乙腈 -5mmol·L-1乙酸盐缓冲液(用醋酸调pH4 5 ),流速 0 5mL·L-1;梯度洗脱;色谱柱:AgilentEclipseXDB-C8, 5μm, 4 6×150mm, 20℃;二极管阵列检测器,检测波长: 204nm。色-质联用中质谱条件为:ESI离子源,负离子模式;气帘气流量1 03×105 Pa,电喷雾电压-4 200V,离子源温度 500℃,辅助雾化气 1 37×105 Pa,干燥气 4 13×105 Pa,相对分子质量检测范围:m/z40~600。液相色谱法测定亚苄基海因和苯丙酮酸的线性相关系数为0 999 05和0 999 86,亚苄基海因和苯丙酮酸的平均回收率为 101 45 %和 97 23 %,相对标准偏差为 1 002%和0 833 8%。精密度以相对标准偏差来表示,分别为0 591 9 % 和0 648 2 %。结果表明,该液相色谱分析方法简便、快速,结果准确,可以用于苯丙酮酸生产的质量控制。     

大豆皂苷Ⅱ的提取及HPLC-MS分析

大豆皂苷是一种生物活性物质,结构不同的大豆皂苷生物活性不同,为了选择性利用B组大豆皂苷,本文考察了B组大豆皂苷的提取、分离方法及B组大豆皂苷Ⅱ的分析方法。采用AB-8大孔吸附树脂柱层析法从脱脂大豆中提取大豆皂苷,并利用硅胶柱层析分离得到B组大豆皂苷,进而通过HPLC-MS法对B组大豆皂苷Ⅱ进行检测。结果表明,本文得出的大豆皂苷提取、分离及检测方法对B组大豆皂苷的选择性应用具有参考价值。     

Determination of Myricetin in Medicinal Plants by High-Performance Liquid Chromatography

The concentrations of myricetin in medicinal plants such as Rosa canina L. (rosa hip), Terebinthina chica L. (terebinth), Urtica dioica L. (nettle), and Portuca oleracea L. (purslane) were determined by high-performance liquid chromatography-mass spectrometry (HPLC-MS). The aglycones of myricetin were extracted using methanol–ascorbic acid– hydrochloric acid, methanol–hydrochloric acid, and methanol, separated within 5 min, and individually quantitated in the positive ionization mode using optimized conditions for HPLC-MS. Methanol–ascorbic acid–hydrochloric acid was the optimum extraction solvent. The myricetin concentration in the plants were between 3 and 58 mg kg^?1, with a limit of quantification equal to 0.1 mg L^?1.     

Pleurotusostreatus and Agaricus subrufescens: investigation of chemical composition and antioxidant properties of these mushrooms cultivated with different handmade and commercial supplements

In this study, the chemical composition, total phenolic content and antioxidant activity (DPPH, ORAC and FRAP assays) of A. subrufescens and P. ostreatus, cultivated with handmade and commercials supplements, were compared. Additionally, the compounds ergosterol, saccharopine, and hexitol were identified in A. subrufescens by HPLC-MS/MS. The antioxidant compound p-coumaric acid and dihexoses was found in both mushroom species. A. subrufescens presented higher total phenolic content (73.8 ± 0.6 mg GAE 100 g⁻¹) and antioxidant activity than P. ostreatus (16.6 ± 0.5 mg GAE 100 g⁻¹). The handmade supplement based on the waste of noble grains presented statistically similar phenolic content to the mushrooms cultivated with commercial ones Spawn Mate II SE (86.1 ± 1.4 and 92.9 ± 0.3 mg GAE 100 g⁻¹, respectively). Therefore, the results support the use of handmade supplements based on agro-wastes as a viable alternative to the use of high-cost commercial ones.     

Simultaneous determination of neonicotinoid insecticides in sunflower-treated seeds (hull and kernel) by LC-MS/MS

A validated analytical method to determine seven neonicotinoids (dinotefuran, nitenpyram, thiamethoxam, clothianidin, imidacloprid, acetamiprid and thiacloprid) in sunflower seeds (hull and kernel) using HPLC coupled to electrospray ionisation mass spectrometry (ESI-MS) is presented. Sample clean-up based on a solid–liquid extraction, and the removal of lipid fraction, in the case of kernels, is proposed and optimised. Low limits of detection and quantification were obtained, ranging from 0.3 × 10^–3 to 1.2 × 10^–3 µg g^–1 and from 1.0 × 10^–3 to 4.0 × 10^–3 µg g^–1, with good precision, and recovery values ranged from 90% to 104% for hulls and kernels. The method was applied for the analysis of five thiamethoxam-dressed sunflower seeds and four non-treated seeds, where, besides thiamethoxam, residues of the other neonicotinoid, clothianidin, were also detected and confirmed via tandem mass spectrometry (LC-ESI-MS/MS). Finally, the presence of residues of thiamethoxam and clothianidin in collected sunflower seeds (hulls) coming from coated seeds confirmed the translocation of these neonicotinoids through the plant up to these seeds.     

Monitoring the presence of residues of tetracyclines in baby food samples by HPLC-MS/MS

Tetracyclin is a group of antimicrobial permitted in animal food production, but their concentrations in food of animal origin should not exceed 100 μg kg⁻¹ (in meat and milk). Although the detection of these substances above these limits involves fines and jail for the producer, residues of tetracyclines are still being detected in food a potential risk to consumer health, especially babies.In the past, baby foods were carefully prepared at homes. However, modern lifestyles have led to the commercialization of ready-made baby food. Generally, these products are made with vegetable and meat from different animals, such as pork, chicken or beef. The presence of tetracyclines in meat at concentrations above 100 μg kg⁻¹ is forbidden in Europe by the Regulation 37/2010. Consequently this concentration is also applicable to the portion of meat present in baby food. Even if the presence of tetracyclines is controlled regularly in meat, they should also be monitored in baby food as babies are vulnerable to such as drugs.A rapid analytical method based on high-performance liquid chromatography coupled to a tandem mass spectrometer (HPLC-MS/MS) for quantification of four tetracyclines (tetracycline, chlortetracycline, doxycycline and oxytetracycline) in baby food is presented. The tetracyclines are extracted with EDTA-McIlvaine buffer, acidified at pH 4.0, followed by liquid–liquid extraction with ethyl acetate. The final extract is analysed within 19 min on a Sunfire HPLC column from Waters. Validation was performed according to the Commission Decision 2002/657/EC. The mean accuracy was 103 μg kg⁻¹, and the mean precision, was less than 23% for all the tetracyclines. The method was tested on 31 prepared baby food samples containing vegetable and beef. The presence of oxytetracycline was detected in one of the samples at a concentration of 5 μg kg⁻¹.     

Determination of phenolic profile and antioxidant activity of pistachio hull using high-performance liquid chromatography–diode array detector–electro-spray ionization–mass spectrometry as affected by ultrasound and microwave

The phytochemicals content and radical scavenging activity of pistachio (Pistacia vera L.) hull extract obtained by different solvents (water, ethanol, and butanol) were measured and compared. Water was selected as superior solvent. Ultrasound-assisted aqueous extraction of the hull by power ultrasound (35 kHz) was more efficient in ascending the phytochemicals content than the sonochemical ultrasonication (130 kHz). High-performance liquid chromatography-mass spectrometry showed increased amounts of vanillic acid, p-coumaric acid, naringenin, and catechin in ultrasound-assisted extracts. Post-extraction sonication declined significantly the phenolics amount and antioxidant property of the aqueous extract. Microwave-assisted extraction increased the phenolics and flavonoids content at extract in a power-dependent trend.     

波生坦片在中国健康受试者中的生物等效性研究

目的:评价中国健康受试者单剂量口服波生坦片受试制剂和参比制剂的人体生物等效性。方法:采用随机、开放、双序列、双周期交叉设计,24例中国健康男性受试者,分别在空腹和餐后情况下,单剂量口服波生坦参比和受试制剂各125 mg。采用高效液相色谱-串联质谱法测定血浆中的波生坦及其活性代谢物羟基波生坦的浓度,以WinNonlin软件按非房室模型计算药代动力学参数,进行生物等效性评价。结果:空腹试验,受试和参比制剂波生坦主要药代动力学参数：Cmax分别为(2.72±1.09)、(2.59±1.02) μg/mL,AUC0-t分别为(13.51±4.55)、(12.61±4.25) μg·mL-1·h,AUC0-∞分别为(14.04±4.46)、 (13.02±4.24) μg·mL-1·h,tmax分别为(3.75±0.81)、(3.98±0.76) h,t1/2分别为(2.70±0.88)、(2.77±0.91) h。餐后试验受试和参比制剂波生坦主要药代动力学参数：Cmax分别为(2.84±0.68)、(2.95±0.99) μg/mL, AUC0-t分别为(14.66±4.27)、(15.34±6.09) μg·mL-1·h, AUC0-∞分别为(15.04±4.41)、(15.68±6.19) μg·mL-1·h,tmax分别为(3.98±1.05)、(3.98±1.21) h,t1/2分别为(2.55±0.65)、(2.71±0.63) h。空腹和餐后试验,两制剂波生坦的AUC0-t、AUC0-∞、Cmax经对数转换后行方差分析,两制剂在给药顺序、制剂间及周期间均无统计学差异(P＞0.05)。在α=0.05水平上行双单侧t检验,AUC0-t、AUC0-∞、Cmax的90%置信区间均在80%～125%的等效区间范围内。结论:波生坦片受试制剂与参比制剂在空腹和餐后条件下均具有生物等效性。