TLC法快速筛查降糖类中成药及保健食品中添加的11种化学药品

目的建立中成药及保健食品中非法添加降糖药的定性检查方法。方法 11种化学降糖药分别采用2个薄层系统检查磺酰脲类降糖药及双胍类降糖药。结果 11种化学降糖药分离良好。结论本方法经济、快速,可用于中成药及保健食品中非法添加降糖类化学药的快速筛查。     

薄层色谱法快速筛查降血糖中成药及保健食品中添加磺酰脲类化学降糖药

目的:建立快速筛查中成药及保健食品中添加磺酰脲类化学降糖药的薄层色谱方法。方法:采用硅胶 GF_(254)薄层板,三氯甲烷-环己烷-乙醇-冰醋酸(8∶12∶1∶1)为展开剂,碘化铋钾试液为显色剂测定。结果:5种磺酰脲类化学降糖药格列喹酮、格列齐特、格列美脲、格列本脲和格列吡嗪呈橙红色斑点,在中成药中的最低检出限分别为每1g 中成药中含0.2,0.3,0.2,0.1,0.2 mg。对16种18个批次的市售降糖中成药及保健食品进行筛查,检出有3种4个批次的降糖中成药及保健食品中分别添加有格列本脲和格列吡嗪。结论:本方法经济、快速简便、灵敏、准确有效。可用于药品检测车上有关中药、保健食品添加化学降糖药的快速筛查。     

保健食品中非法添加酚酞的快速检测方法

目的建立一种保健食品中非法添加酚酞的快速检测方法。方法选用一般化学显色和薄层色谱法对保健食品中非法添加酚酞进行快速筛查。结果该法可对保健食品中非法添加酚酞进行定性和定量测定。结论该方法可适用于大批量保健食品的快速检验工作。     

减肥类保健食品中非法添加盐酸西布曲明的快速检测

目的建立检测减肥类保健食品中非法添加盐酸西布曲明的快速定性检测方法。方法采用薄层色谱法、高效液相色谱-二极管阵列检测器法进行定性鉴别,并采用高效液相色谱法测定其中盐酸西布曲明的含量。结果在试验的10种市售样品(含赠品)中,其中8个品种(含赠品)中被检测到掺有盐酸西布曲明。结论该方法选择性强、灵敏度高,可作为分析检测减肥类保健食品中非法添加盐酸西布曲明的比较有效的方法。     

两种快速检测降糖类中成药中添加磺酰脲类药物方法的比较

目的比较快速检验降糖类中成药中是否添加磺酰脲类化学成分的薄层色谱（TLC）法和试管反应法。方法采用TLC法和试管反应法分别检测药品中是否含有磺酰脲类化学成分,并用液相质谱联用（LC—MS）法作最终判断结果。结果两种方法差异性较大,TLC法专属性较差,容易出现假阳性;试管反应法灵敏度高,分析成本低,专属性强,试验结果明显,现象易观察。结论试管反应法非常适宜于现场检测降糖类中成药和保健食品中是否添加了磺酰脲类化学药物,对于保障药品质量和用药安全具有重要意义。     

降糖保健食品中非法添加盐酸苯乙双胍和格列本脲的检测

目的:建立检测降糖保健食品中非法添加化学成分盐酸苯乙双胍和格列本脲的定性、定量检测方法.方法:采用薄层色谱法、高效液相色谱-二极管阵列检测法、LC/MS/MS联用技术进行定性鉴别,并采用高效液相色谱法测定其中盐酸苯乙双胍和格列本脲的含量.结果:在抽取的9种市售样品中,有3种检出了盐酸苯乙双胍和格列本脲,1#～3#阳性样品中添加的盐酸苯乙双胍和格列本脲分别为8.54、6.51、10.53 mg/g和6.01、4.04、2.70 mg/g.结论:该方法快速、准确、灵敏、可靠,可用于有效监测保健食品中非法添加的盐酸苯乙双胍和格列本脲.     

减肥类保健食品中非法添加化学药物检测技术和方法的研究进展

目的:为减肥类保健食品中非法添加化学药物的检测提供参考。方法:查阅国内外相关文献,对近年来减肥类保健食品中非法添加化学药物的概况以及检测技术和方法研究情况进行归纳和总结。结果与结论:减肥类保健食品中非法添加的化学药物有食欲抑制剂类、胃肠道脂肪酶抑制剂类、利尿药类、能量消耗剂类、泻药类、降糖药类等。涉及的检测技术和方法包括理化鉴别法、红外光谱法、拉曼光谱法、核磁共振氢谱法、薄层色谱法、质谱法、液相色谱法、液相色谱-质谱联用法、气相色谱-质谱联用法和离子迁移谱法等。保健食品中非法添加化学药物检测水平的提高以及相应检测标准和指南的建立和完善,有利于更好地打击相关非法行为,保障消费者的合法权益和身体健康。     

薄层色谱-显微红外光谱(TLC-Micro IR)联用技术检测减肥保健食品中非法添加盐酸芬氟拉明

目的: 建立减肥保健食品中非法添加盐酸芬氟拉明的定性检测方法。方法: 供试品用甲醇超声提取, 以硅胶GF₂₅₄铝合金薄层板(5 cm×10 cm)为固定相, 以三氧甲烷-甲醇-氨水(11:1:0.12)为展开剂, 在紫外灯254 nm下检视, 用薄层色谱法(TLC)快速初筛后, 再联用显微红外光谱法(Micro IR)对其进行定性检测。结果: 在检查下的9批供试品中有2批含有盐酸芬氟拉明。结论: 所建立的方法专属性强、灵敏度高、重现性好, 可以作为该类保健食品非法添加盐酸芬氟拉明的快速检测方法。     

UPLC-MS/MS法快速检测减肥类保健食品中5种非法添加化学成分

目的建立专属、灵敏的UPLC-MS/MS方法用于快速定性定量检测减肥类保健食品中5种非法添加化学成分。方法供试样品经甲醇提取后,采用超高效液相色谱-串联质谱法(UPLC-MS/MS),以BEH-C18为分析柱,流动相采用含0.1%冰醋酸的20mmol/L醋酸铵水溶液和甲醇进行梯度洗脱,电喷雾电离(ESI)、多重反应监测(MRM)扫描模式,对保健食品中非法添加的盐酸西布曲明、酚酞、盐酸芬氟拉明、咖啡因、呋塞米等5种化学成分进行快速定性定量检测。结果所建立方法能快速定性定量检测保健食品中5种非法添加化学药物成分,5种成分在6min内完全分离,且线性良好,平均加样回收率在97.7%~100.7%,方法检出限为0.0025~0.0075mg/g。结论所建方法快速、灵敏、专属性强,适用于减肥类保健食品中非法添加化学成分的快速定性定量检测。     

中成药、保健食品中非法添加诺氟沙星的快速检测方法研究

目的建立一种简单、快速、准确的检验方法鉴别、筛查出治疗前列腺疾病的中成药及保健食品中是否非法添加诺氟沙星药物。方法采用薄层色谱法（TLC）、高效液相色谱法（HPLC）等检测方法对治疗前列腺疾病的中成药及保健食品中非法添加诺氟沙星抗生素进行快速鉴别、分析研究。结果能准确筛查出治疗前列腺疾病的中成药及保健食品中非法添加的诺氟沙星抗生素成分。结论建立的检测方法简单、快速、准确,能应用于这一类假劣药品的日常监督、快速分析。     

Treatment of type 2 diabetes: inadequate assessment of oral antidiabetic combinations

(1) Metformin and glibenclamide are the only oral antidiabetics with a proven impact on the complications of type 2 diabetes. (2) Treatment with one of these drugs often fails to achieve the recommended target in HbA1c level (below 7%). (3) Only one randomised trial has assessed the preventive efficacy of a combination of oral antidiabetics when hyperglycaemia persists despite treatment with a glucose-lowering sulphonylurea. The trial showed that combining metformin and a glucose-lowering sulphonylurea is associated with a higher mortality than therapy with a sulphonylurea alone. (4) Despite this result, most clinical guidelines recommend the metformin + glucose-lowering sulphonylurea combination when oral antidiabetic monotherapy fails. (5) In the absence of convincing data supporting any particular strategy, all options should be discussed with patients including continuing with oral antidiabetic monotherapy, or starting insulin.     

Non insulin-dependent diabetes mellitus (type 2) secondary failure. Metformin-glibenclamide treatment

The goal of sulphonylurea (S) treatment in Non-Insulin-Dependent Diabetes Mellitus (NIDDM - type 2 diabetes) subjects should be to obtain a satisfactory glycemic control (fasting glycemic levels < 140 mg%). The loss of an adequate blood glucose control after an initial variable period of S is known as secondary failure (SF). The number of SF are extremely variable among different trials for many reasons, some of which are patient-related: increased food intake, weight gain, non-compliance, poor physical activity, stress, diseases and÷or impaired pancreatic beta cell function, desensitization after S chronic therapy, reduced absorption, concomitant therapies. Many therapeutic strategies have been proposed to achieve an adequate metabolic control in type 2 diabetes patients: switch to intensive insulin therapy and subsequent return to S therapy; association with insulin; association with sulphonylureas plus biguanides. The association biguanides and S, in particular glibenclamide plus metformin, is now widely used by diabetologists in SF since glibenclamide improves insulin secretion while metformin exerts its antidiabetic.     

Analysis of the oral hypoglycemic agent, glibenclamide, in a health food

Glibenclamide, a sulfonylurea derivative (SU) antidiabetic agent was detected in a health food by three different methods: TLC, HPLC, and liquid chromatography-mass spectrometry (LC-MS). For analysis of SU antidiabetics, the sample was extracted with acetone as a sample solution. TLC analysis of the sample solution showed a specific spot that had the same characteristics as those of glibenclamide standard solution. HPLC analysis monitored using a photo-diode array detector showed that the sample solution had a peak with a unique UV spectrum, with coincided with that of standard glibenclamide. In sample solution, LC-MS analysis in positive and negative modes indicated that the (M + H)+ and (M - H)- ions occurred at m/z 494 and m/z 492, respectively. These results indicate that the monoisotopic mass is 493, coincident with that of glibenclamide. Quantitative HPLC analysis showed that the glibenclamide content in the health food was 0.78 mg/capsule (1.55 mg/g of sample contents). Because the initial dosage of glibenclamide for diabetics is 1.25-2.5 mg per day, this health food has sufficient medicinal effect and also has the potential to cause adverse effects.     

Antidiabetic sulphonylureas activate mitochondrial permeability transition in rat skeletal muscle

Antidiabetic sulphonylureas can bind to various intracellular organelles including mitochondria. The aim of this study was to monitor the influence of antidiabetic sulphonylureas on membrane permeability in mitochondria isolated from rat skeletal muscle. The effects of glibenclamide (and other sulphonylurea derivatives) on mitochondrial function were studied by measuring mitochondrial swelling, mitochondrial membrane potential, respiration rate and Ca2+ transport into mitochondria. We observed that glibenclamide induced mitochondrial swelling (EC50 = 8.2 +/- 2.5 microM), decreased the mitochondrial membrane potential and evoked Ca2+ efflux from the mitochondrial matrix. These effects were blocked by 2 microM cyclosporin A, an inhibitor of the mitochondrial permeability transition. Moreover, 30 microM glibenclamide accelerated the respiratory rate in the presence of glutamate/malate, substrates of complex I of the mitochondrial respiratory chain. In conclusion, we postulate that the antidiabetic sulphonylureas activate the mitochondrial permeability transition in skeletal muscle by increasing its sensitivity to Ca2+.     

The in vivo interaction between gliclazide and glibenclamide and insulin on glucose disposal in the rat.

Many reports suggest that extrapancreatic actions contribute to the antidiabetic effect of sulphonylurea drugs (SUs). In this work, the ability of two SUs, namely, gliclazide and glibenclamide, to augment insulin action was studied in vivo. Both drugs elevated the plasma concentration of immunoreactive insulin (IRI) and lowered the plasma concentrations of glucose and non-esterified fatty acids (NEFA) in normal intact rats. These changes were not reproduced in alloxan-diabetic or eviscerated rats. The actions of insulin on plasma glucose and NEFA were not augmented by gliclazide in alloxan-diabetic rats. Neither gliclazide nor glibenclamide (given acutely and for 30 days) augmented the actions of exogenously administered insulin in reducing plasma glucose or NEFA concentrations in intact or eviscerated animals. It was concluded that these SUs do not produce their acute or chronic effects on blood glucose by augmenting the actions of insulin.     

Physicochemical interactions of metformin hydrochloride and glibenclamide with several health foods

In this study, as an approach to possible pharmacokinetic interactions between antidiabetic agents and health foods, we investigated the binding of metformin and glibenclamide to aojiru, kurosu, and blueberry extract using a dialysis method. The permeation of metformin from the inner to the outer side of the dialysis tube during 90 min was not altered in the presence of aojiru or kurosu, and slightly decreased by 20% compared with the control in the presence of blueberry extract, indicating that the interactions between metformin and these three health foods are limited. On the other hand, when these three health foods were added to inner medium together with glibenclamide, they significantly lowered the outer glibenclamide concentrations. The magnitude of the decrease in the outer glibenclamide concentrations was the most extensive in the presence of kurosu (60%), followed by aojiru (36%) and blueberry extract (45%). The present results suggest that metformin and glibenclamide interact differently with aojiru, kurosu, and blueberry extract and that these three health foods might modulate the absorption of glibenclamide in vivo.     

HPLC法检测降糖中药制剂中非法添加的格列本脲

目的建立降糖中药制剂中所添加的格列本脲的定性、定量检测方法。方法采用高效液相色谱法。色谱柱:C18柱(4.6 mm×250 mm,5μm);流动相:0.1 mol·L-1磷酸二氢钾-乙腈(53∶47);流速1.0 mL·min-1;柱温35℃;检测波长300 nm。结果 1种供试品中检出格列本脲。格列本脲浓度在0.051～1.014 4 mg·mL-1范围内,峰面积与进样量呈良好的线性关系,相关系数r=1.000,平均回收率为99.97%,RSD为1.3%。结论本方法简便易行、准确可靠,可作为监测降糖中药制剂非法添加格列本脲的有效方法。     

中药保健品中非法掺入格列本脲的检测

目的:建立中药保健品中非法掺入化学成分格列本脲的定性、定量检测方法,为药监、药检部门提供参考。方法:采用薄层色谱法、高效液相色谱法对怀疑掺有格列本脲的荞芪胶囊的提取物进行分离分析,并采用高效液相色谱-二级管阵列检测法及直接电喷雾四级杆质谱技术对其进行定性鉴别,另采用高效液相色谱法测定其中格列本脲的含量。结果:供试品荞芪胶囊A、荞芪胶囊B均检出格列本脲,其含量分别为1·51、0·55mg/粒。结论:本方法专属性强、灵敏度高、操作简便,可作为监测掺有格列本脲中药保健品的有效方法。     

The sulphonylurea glibenclamide inhibits multidrug resistance protein (MRP1) activity in human lung cancer cells

1. Glibenclamide, a sulphonylurea widely used for the treatment of non-insulin-dependent diabetes mellitus, has been shown to inhibit the activities of various ATP-binding cassette (ABC) transporters. In the present study, its effects towards multidrug resistance protein 1 (MRP1), an ABC efflux pump conferring multidrug resistance and handling organic anions, were investigated. 2. Intracellular accumulation of calcein, an anionic dye substrate for MRP1, was strongly increased by glibenclamide in a dose-dependent manner in MRP1-overexpressing lung tumour GLC4/Sb30 cells through inhibition of MRP1-related calcein efflux. By contrast, glibenclamide did not alter calcein levels in parental control GLC4 cells. Another sulphonylurea, tolbutamide, was however without effect on calcein accumulation in both GLC4/Sb30 and GLC4 cells. 3. Glibenclamide used at 12.5 microM was, moreover, found to strongly enhance the sensitivity of GLC4/Sb30 cells towards vincristine, an anticancer drug handled by MRP1. 4. Efflux of carboxy-2',7'-dichlorofluorescein, an anionic dye handled by the ABC transporter MRP2 sharing numerous substrates with MRP1 and expressed at high levels in liver, was also strongly inhibited by glibenclamide in isolated rat hepatocytes. 5. In summary, glibenclamide reversed MRP1-mediated drug resistance likely through inhibiting MRP1 activity and blocked organic anion efflux from MRP2-expressing hepatocytes. Such effects associated with the known inhibitory properties of glibenclamide towards various others ABC proteins suggest that this sulphonylurea is a general inhibitor of ABC transporters.     

Desensitization of sulphonylurea- and nutrient-induced insulin secretion following prolonged treatment with glibenclamide

Functional effects of prolonged exposure to the sulphonylurea glibenclamide were examined in a popular clonal pancreatic beta-cell line, denoted as BRIN-BD11. In acute 20-min incubations, 200 microM of tolbutamide or glibenclamide stimulated insulin release from non-depolarized and depolarized cells, which was dramatically reduced following 18-h culture with 100 microM glibenclamide. Sulphonylurea desensitization in non-depolarized cells was reversed following 6-36-h subsequent culture in the absence of glibenclamide. However, desensitization of insulinotropic effects of sulphonylureas in depolarized cells following glibenclamide culture and associated decline in cellular insulin content was not fully reversible. Culture with 100 microM glibenclamide also markedly reduced the acute insulinotropic actions of glucose, L-alanine, L-arginine, 2-ketoisocaproic acid (KIC) and KCl. These effects were almost completely reversed following 18-h culture in the absence of the sulphonylurea.