中药保健品中他达拉非的检测

目的:建立测定中药保健品中掺入化学药他达拉非的方法。方法:采用高效液相色谱-质谱联用法对两种样品进行了色谱分离及质谱鉴定。结果:两样品中检测物质的色谱行为,与质谱行为,均与他达拉非对照药品一致,表明两种胶囊样品中均含有他达拉非。结论:方法简便,快速,专属性好,适用于中药保健品中他达拉非的检测。     

中成药与保健品中非法添加化学药物的检测方法

（1. ［摘要］在中成药及保健品等制剂中非法添加化学药物是当前不法分子常用的制假手段之一,目前主要检测方法有化学反应法、薄层色谱法、高效液相色谱法、液相色谱 质谱联用法、高效毛细管电泳法、红外光谱法等。这些方法的应用为相关部门的打假工作提供了强有力的技术保障。作者就近几年来有关中成药及保健品中非法添加化学药物的检测方法作了综述。     

灵芝成分测定方法研究进展

随着检测技术不断发展,灵芝有效成分的测定方法也不断更新和完善.本文根据灵芝活性成分的不同,分几个方面对其检测技术的应用进展情况做一综述.检测方法主要有近红外光谱和化学计量学方法、高效液相色谱指纹图谱法、高效液相色谱-电喷雾-质谱(HPLC-ESI-MS)法,荧光光谱法、MALDI-TOF-MS、苯酚-硫酸比色法、紫外分光光度法、柱前衍生化-HPLC法、氨基酸分析法、氢化物-原子荧光光谱法、毛细管电泳-质谱联用法、超高效液相色谱-串联质、气相色谱分析-质谱法分析、质谱和核磁共振方法、LC-QTOF-MS飞行时间质谱法、超高效液相色谱单四极质谱以及多项检测技术的联合应用等.     

中药制剂中非法掺入化学药物的研究近况

目的：近年来中药制剂中非法添加功效相似的化学药物时有发生，目前从中鉴别检查化学药物的方法主要有：薄层色谱法、高效液相色谱法、液相色谱-质谱联用法、高效毛细管电泳法、红外光谱法，这些研究为制定相应的技术检验标准提供了依据。     

液相色谱-串联四极杆质谱联用法测定减肥类药品及保健品中非法掺入酚酞的研究

目的：建立检测减肥类药品及保健品中非法掺入酚酞的专属性方法。方法：采用液相色谱-串联四极杆质谱联用法。通过相对分子质量、二级质谱碎片信息、液相色谱保留时间和紫外光谱四方面信息，对减肥类药品及保健品的提取液进行液相色谱-串联四极杆质谱分析。通过与对照品的光谱、色谱及质谱行为相比较，对减肥类药品及保健品中非法掺入的酚酞进行定性鉴别。结果：在114种受试减肥类药品及保健品中，42种被检测到掺有酚酞。结论：该方法选择性强，灵敏度高，可作为分析检测非法减肥类药品及保健品中酚酞的比较有效的方法。     

补肾壮阳类药品中非法添加化学药物检测技术的研究进展

目的了解补肾壮阳类中成药和保健品中非法添加化学药物检测技术的研究进展。方法通过查阅相关文献和分析总结,对近年来补肾壮阳类中成药和保健品中非法添加化学药物检测技术的研究进展进行综述。结果补肾壮阳类中成药和保健品中非法添加的化学药物包括磷酸二酯酶-5抑制剂、蛋白同化制剂、α-肾上腺素受体阻滞剂、多巴胺受体激动剂和天然前列腺素类物质等。涉及的检测方法包括理化分析法、薄层色谱法、高效液相色谱法、液相色谱-质谱联用技术、直接实时分析-MS/MS法、中空纤维膜液相微萃取-车载HPLC法、离子迁移谱法、显微共聚焦拉曼光谱法和近红外光谱法等。结论补肾壮阳类中成药和保健品中非法添加化学药物的检测技术取得了一定进展。不断发展检测技术是一方面,从多方面加强监管也非常重要。     

中药注射剂中吐温80的定性定量测定研究

目的：测定14种中药注射剂中吐温80的含量。方法：联合采用比色法、高效液相色谱-蒸发光散射检测法和液相色谱-质谱联用法定性判定中药注射液中是否含有吐温80,采用高效液相色谱-蒸发光散射检测法测定吐温80的含量。结果：14种中药注射剂（其中3种中药注射剂厂家称未添加吐温80）中均含有吐温80,含量范围0．18％～0．57％。结论：中药注射剂中吐温80的添加有待进一步监督与规范。     

液相色谱-串联四极杆质谱联用法测定中药降糖制剂中掺入罗格列酮的研究

目的:建立检测中药降糖制剂中非法掺入的罗格列酮专属性方法。方法:采用液相色谱-串联四极杆质谱联用法。通过相对分子质量、二级质谱碎片信息、液相色谱保留时间和紫外光谱四方面信息,对中药降糖制剂的提取液进行液相色谱-串联四极杆质谱分析。通过与对照品的光谱、色谱及质谱行为相比较,对中药降糖制剂中非法掺入的合成降糖药进行定性鉴别。结果:在4种受试中药降糖制剂中,2种被检测到掺有罗格列酮。结论:该方法选择性强,灵敏度高,可作为分析检测中药降糖制剂中非法掺入罗格列酮的比较有效的方法。     

人体生物样本常用分析方法

目前常用的几种分析方法归纳如下。 色谱法:气相色谱法(GC)、高效液相色谱法(HPLC)、色谱-质谱联用法(LC-MS、LC-MS-MS,GC-MS,GC-MS-MS)等,可用于大多数药物的检测。 免疫学方法法:放射免疫分析法、酶免疫分析法、     

液相色谱-质谱联用法检测非法制剂中的布洛芬

目的采用液相色谱-质谱联用法检测非法制剂中的布洛芬。方法选用Venusil MPC18色谱柱(150mm×4.6mm,5μm),以0.01mol/L醋酸铵溶液(含0.1%的三乙胺,用冰醋酸调pH至3.5)-乙腈(47:53)为流动相,对非法制剂的提取液进行液相色谱-质谱分析。结果通过比较对照品的色谱、紫外光谱及质谱行为,对非法生产的制剂进行定量测定和定性鉴别,在待检非法制剂中均检出了布洛芬。结论液相色谱-质谱联用法选择性强,灵敏度高,可用于分析检测非法制剂中的布洛芬。     

Pharmacokinetic herb-drug interactions (part 1): origins, mechanisms, and the impact of botanical dietary supplements

Phytochemicals have been components of man's diet for millennia and are believed to have played a significant role in steering the functional development of xenobiotic metabolizing enzymes and transporters within the human gastrointestinal tract. Only recently, however, have plant secondary metabolites been recognized as modulators of human drug disposition. Despite exposure to thousands of structurally diverse dietary phytochemicals, only a few appear to significantly modulate human drug metabolizing enzymes and transporters. In some instances, these interactions may have beneficial effects like cancer prevention, whereas others may dramatically affect the pharmacokinetics of concomitantly administered drugs. In today's global economy, the opportunity for exposure to more exotic phytochemicals is significantly enhanced. Formulated as concentrated phytochemical extracts, botanical dietary supplements are vehicles for a host of plant secondary metabolites rarely encountered in the normal diet. When taken with conventional medications, botanical dietary supplements may give rise to clinically significant herb-drug interactions. These interactions stem from phytochemical-mediated induction and/or inhibition of human drug metabolizing enzymes and transporters.     

Pharmacokinetic herb-drug interactions (part 2): drug interactions involving popular botanical dietary supplements and their clinical relevance

In Part 2 of this review, a critical examination of the pertinent scientific literature is undertaken in order to assess the interaction risk that popular dietary supplements may pose when taken concomitantly with conventional medications. Botanicals most likely to produce clinically important herb-drug interactions are those whose phytochemicals act as mechanism-based inhibitors of cytochrome P450 enzyme activity (e.g., HYDRASTIS CANADENSIS, PIPER NIGRUM, SCHISANDRA CHINENSIS) or function as ligands for orphan nuclear receptors (e.g., HYPERICUM PERFORATUM). In addition, several external factors unrelated to phytochemical pharmacology can augment the drug interaction potential of botanical supplements.     

Identification of botanicals and potential contaminants through RFLP and sequencing

Botanical supplements for health enhancement are being increasingly used in the United States, but no safeguards are formally in place to ensure that they are not contaminated with non-efficacious or potentially harmful plant material. A molecular approach, which allows the authentication of botanical ingredients and detection of contaminating plant material by analyzing the ITS-1 region by PCR-RFLP and subsequent sequencing, is described. When using starting material from which DNA can be obtained, this method has the potential for identifying both primary and contaminating plant material in botanical dietary supplements.     

Evaluation of commercial ginkgo and echinacea dietary supplements for colchicine using liquid chromatography-tandem mass spectrometry

In response to concerns that commercial dietary supplements containing Ginkgo biloba (ginkgo) and Echinacea purpurea, Echinacea angustifolia, or Echinacea pallida (echinacea) might be contaminated with colchicine, a highly selective and sensitive assay was developed for colchicine that is based on high-performance liquid chromatography-tandem mass spectrometry (LC-MS-MS). The method utilizes reversed-phase HPLC separation of compounds in a methanolic extract of the dietary supplement or botanical sample followed by positive ion electrospray ionization with collision-induced dissociation and multiple reaction monitoring of three characteristic fragmentation pathways of the protonated molecule of colchicine, m/z 400 --> 358, 400 --> 326, and 400 --> 310. The minimal detectable concentration of colchicine using this assay was 10 pg on-column, which is equivalent to 20 ppb colchicine in a 0.5 g ginkgo leaf sample. The method was validated by analyzing 0.5 g samples spiked with colchicine and determining the recovery. A total of 26 commercial ginkgo and echinacea dietary supplements were purchased from pharmacies in Chicago, IL, and analyzed for colchicine. In contrast to a recent report, no colchicine was detected in any of the samples. In addition, authenticated ginkgo leaves were collected, assayed, and found to contain no colchicine, which is consistent with the botanical literature. On the basis of the results obtained using this new LC-MS-MS assay, which is more sensitive and more selective than previously published methods for colchicine, we find no cause for concern regarding colchicine contamination of ginkgo or echinacea dietary supplements.     

Compounding botanicals: a legal perspective.

OBJECTIVE: To describe the effects of the new law, section 503A, "Pharmacy Compounding," of the Federal Food, Drug, and Cosmetic Act on the compounding of drugs, dietary supplements, and cosmetics. DATA SOURCES: The Food and Drug Administration (FDA) Modernization Act of 1997; Federal, Food, Drug, and Cosmetic Act; Code of Federal Regulations; Federal Register; Food and Drug Administration Guidances. DATA SYNTHESIS: Pharmacy compounding, which traditionally is considered part of pharmacy practice and is regulated by the states, has been confused with drug manufacturing, an activity regulated by FDA. Section 503A, "Pharmacy Compounding," was enacted as part of the Food and Drug Administration Modernization Act of 1997 to distinguish compounding from manufacturing. This law addresses the compounding of drug products, but not necessarily the compounding of botanicals, which may be considered dietary supplements, cosmetics, or drugs. CONCLUSION: Section 503A applies to the compounding of products intended for a drug use, but does not apply to compounded products that are intended for dietary supplement or cosmetic use. Compounded dietary supplements and cosmetics must instead adhere to relevant federal requirements, including those for good manufacturing practices and labeling.     

Screening botanical extracts for quinoid metabolites.

Botanical dietary supplements represent a significant share of the growing market for alternative medicine in the USA, where current regulations do not require assessment of their safety. To help ensure the safety of such products, an in vitro assay using pulsed ultrafiltration and LC-MS-MS has been developed to screen botanical extracts for the formation of electrophilic and potentially toxic quinoid species upon bioactivation by hepatic cytochromes P450. Rat liver microsomes were trapped in a flow-through chamber by an ultrafiltration membrane, and samples containing botanical extracts, GSH and NADP(H), were flow-injected into the chamber. Botanical compounds that were metabolized to reactive intermediates formed stable GSH adducts mimicking a common in vivo detoxification pathway. If present in the ultrafiltrate, GSH conjugates were detected using LC-MS-MS with precursor ion scanning followed by additional characterization using product ion scanning and comparison to standard compounds. As expected, no GSH adducts of reactive metabolites were found in extracts of Trifolium pratense L. (red clover), which are under investigation as botanical dietary supplements for the management of menopause. However, extracts of Sassafras albidum (Nutt.) Nees (sassafras), Symphytum officinale L. (comfrey), and Rosmarinus officinalis L. (rosemary), all of which are known to contain compounds that are either carcinogenic or toxic to mammals, produced GSH adducts during this screening assay. Several compounds that formed GSH conjugates including novel metabolites of rosmarinic acid were identified using database searching and additional LC-MS-MS studies. This assay should be useful as a preliminary toxicity screen during the development of botanical dietary supplements. A positive test suggests that additional toxicological studies are warranted before human consumption of a botanical product.     

Chemical and biological characterization and clinical evaluation of botanical dietary supplements: a phase I red clover extract as a model

Botanical dietary supplements, as compared with nutritional supplements or single-component pharmaceutical drugs, are typically less-refined preparations derived from bulk plant material and, as such, require a modified approach to their development, production, and evaluation. An integrated, multidisciplinary team of scientific and clinical investigators is required in order to develop high quality phytomedicines and rigorously evaluate their safety and efficacy. Research on botanicals involves unique challenges as plant source materials frequently vary in chemical content and may contain unwanted pesticides, heavy metals, contaminant plant species, or other adulterants. Ideally, a botanical formulation should be standardized, both chemically and biologically, by a combination of analytical techniques and bioassays. This combination approach provides multiple measures by which reproducible quality and efficacy of botanical supplements may be achieved, and is particularly useful for botanical products for which the active compound(s) have not yet been identified. Safety and toxicity should be evaluated during the supplement development process in both in vitro and in vivo systems. A number of liquid chromatography-mass spectrometry methods can aid in the assessment of purity, bioavailability, toxicity, metabolism, and molecular target profiling of botanical extracts. Clinical investigators must appreciate the complexity of multi-component phytomedicines and adjust trial protocols accordingly. This review highlights practical considerations of value to basic science and clinical investigators engaged in the study of botanical supplements. Lessons and examples are drawn from the authors' experience in designing and developing a red clover (Trifolium pratense L.) standardized extract for evaluation in Phase I and Phase II clinical trials.     

Determination of ephedra alkaloid and caffeine concentrations in dietary supplements and biological fluids

Dietary supplements containing botanical forms of caffeine and ephedra alkaloids have been widely promoted and used in the U.S. for weight loss and athletic enhancement despite a lack of adequate research on the pharmacology of these botanical stimulants. In order to analyze dietary supplements and perform human pharmacokinetic studies, an analytical approach with good precision and accuracy was needed with sufficient sensitivity to detect very low levels of ephedra alkaloids. A liquid chromatography-atmospheric pressure chemical ionization (APCI) tandem mass spectrometry (LC-MS-MS) method was developed for quantitating the various ephedrine-group alkaloids found in dietary supplements that contain Ephedra species, and in plasma and urine of persons consuming these supplements. Using this method, low nanogram-per-milliliter concentrations of ephedrine, pseudoephedrine, norephedrine, norpseudoephedrine, methylephedrine, methylpseudoephedrine, and caffeine can be quantitated in a 12-min LC-MS-MS run.