超高液相色谱法测定桔梗饮片和桔梗配方颗粒中桔梗皂苷D含量

目的 采用超高效液相色谱法建立桔梗饮片及桔梗配方颗粒中桔梗皂苷D的含量测量方法,为桔梗配方颗粒的质量控制提供实验依据。 方法 采用Waters Acquity UPLC HSS T3柱（2.1 mm×50 mm,μm）,以乙腈和水为流动相,梯度洗脱,流速 0.25 mL/min,检测波长210 nm,柱温29 ℃。 结果 桔梗皂苷D进样量在0.504~2.520 μg范围内与峰面积的线性关系良好,平均加样回收率为99.89%,RSD为1.64%;桔梗饮片和桔梗配方颗粒中桔梗皂苷D的含量具有差异。 结论 本实验所建立的测定方法简便、准确、可靠,可用于桔梗饮片和桔梗配方颗粒中桔梗皂苷D含量的检测。     

Identification of furosemide in hair in a post‐mortem case by UHPLC‐MS/MS with guidance on interpretation

Testing for drugs in hair raises several difficulties. Among them is the interpretation of the final concentration(s). In a post‐mortem case, analyses revealed the presence of furosemide (12 ng/mL) in femoral blood, although it was not part of the victim's treatment. The prosecutor requested our laboratory to undertake an additional analysis in hair to obtain information about the use of furosemide. A specific method was therefore developed and validated to identify and quantify furosemide in hair by UHPLC‐MS/MS. After decontamination of 30 mg of hair, incubation in acidic condition, extraction with ethyl acetate, the samples were analyzed by UHPLC‐MS/MS. Furosemide was found in the victim's hair at 225 pg/mg. However, it was not possible to interpret this concentration due to the absence of data in the literature. Therefore, the authors performed a controlled study in two parts. In order to establish the basis of interpretation, several volunteers were tested (four after a single 20 mg administration and twenty‐four under daily treatment). The first part indicated that a single dose is not detectable in hair using our method. The second part demonstrated concentrations ranging from 5 to 1110 pg/mg with no correlation between dosage and hair concentrations. The decedent's hair result was interpreted as repeated exposures. In the case of furosemide analysis, hair can provide information about its presence but cannot give information about dosage or frequency of use.     

Analysis of thin-layer chromatograms of paint pigments and dyes by direct microspectrophotometry

The Nanospec 10S microspectrophotometer has been used to produce reflectance spectra over the 380–900 nm range from coloured thin-layer chromatography spots. The method has been applied to extracted paint pigments and to dyes from other materials examined in forensic science.     

苦地胆内酯类化合物的制备及其体外抑菌效果研究

为探讨中药苦地胆有效成分苦地胆内酯的抗菌效果,用浓度为800mL/L的乙醇溶液进行热回流浸提,制备苦地胆内酯的粗提物,经硅胶柱层析分离、纯化,再结晶,制得苦地胆内酯类化合物,用薄层层析法进行苦地胆内酯检测与鉴定,并进行了苦地胆内酯类化合物的体外抑菌试验。结果显示,当浓度为2.0mg/mL时,苦地胆内酯类化合物对巴氏杆菌、蜡状芽孢杆菌具有明显的抑制作用(P0.05),对金黄色葡萄球菌、肠炎沙门氏菌和鸡大肠杆菌呈现极明显的抑制作用(P0.01);浓度分别为50、10mg/mL时,苦地胆内酯类化合物对5种供试菌均有极明显的抑制作用(P0.01)。苦地胆内酯类化合物对供试金黄色葡萄球菌、肠炎沙门氏菌、巴氏杆菌、鸡大肠杆菌、蜡状芽孢杆菌的最小抑菌浓度分别为0.313、0.313、0.156、0.625mg/mL和1.25mg/mL;对蜡状芽孢杆菌的最小杀菌浓度为2.5mg/mL,对其他4种供试菌的最小杀菌浓度均为0.625mg/mL。表明,苦地胆内酯类化合物具有很好的体外抗菌效果。     

益肾蠲痛口服液治疗绝经后骨质疏松症临床观察

目的 观察益肾蠲痛口服液治疗肾阳虚型绝经后骨质疏松症（postmenopausal osteoporosis,PMOP）的临床疗效。方法 将120例肾阳虚型PMOP患者随机分为治疗组和对照组,每组60例。两组患者均口服钙尔奇,治疗组患者加服益肾蠲痛口服液,对照组患者加服骨康口服液,疗程均为12个月,随访24个月。治疗前后及随访时,分别采用视觉模拟评分法（visual analogue scale,VAS）评价腰背疼痛,采用双能X线检测骨密度（bone mineral density,BMD）;并观察两组中医证候疗效及脆性骨折发生情况。结果 治疗后,两组VAS评分均较治疗前显著降低（P<0.01）;腰椎、股骨颈、Ward三角BMD均较治疗前显著上升（P<0.01）;随访时,治疗组VAS下降值及腰椎（L2—4）、股骨颈、Ward三角BMD升高值均显著大于对照组（P<0.01）。两组中医证候疗效及脆性骨折复发率比较,差异均无统计学意义（P>0.05）。结论 益肾蠲痛口服液可减轻PMOP患者腰背疼痛,提高BMD,改善中医症状,防止脆性骨折复发,在减轻腰背疼痛和提高BMD方面较对照药具有明显优势。     

液相色谱-质谱联用法测定复方氨酚烷胺胶囊人体生物等效性

目的 研究复方氨酚烷胺胶囊的人体生物等效性。方法 采用双周期交叉实验设计,22名健康男性受试者随机交叉单剂量口服复方氨酚烷胺胶囊试验制剂和参比制剂各1粒。采用液相色谱-质谱联用法测定血浆中对乙酰氨基酚（paracetamol, PAR）、金刚烷胺（amantadine, AMA）、马来酸氯苯那敏（chlorphenamine, CHL）和咖啡因（caffenine, CAF）的浓度,采用DAS3.2.5软件计算药物代谢动力学参数,并采用双侧t检验法和90%置信区间比较主要药物代谢动力学参数（cmax,tmax,t1/2和AUC0-t）。结果 受试制剂和参比制剂中PAR、AMA、CAF和CHL的AUC0→t、AUC0→∞、cmax和tmax比较,差异均无统计学意义（P>0.05）。结论 本实验方法准确、灵敏、简便,两种制剂具有生物等效性。     

歙白术与其他产地白术中白术内酯类成分含量比较

目的 以白术内酯类成分为评价指标,比较歙白术与其他产地白术的质量差异。方法 采用高效液相色谱法同时测定安徽、浙江5个产地白术药材中白术内酯Ⅰ、Ⅱ、Ⅲ的含量。色谱柱：Agilent TC-C18(4.6 mm×250 mm,5 μm);流动相：甲醇-水(70∶30);检测波长：白术内酯Ⅰ、Ⅲ的检测波长为220 nm,白术内酯Ⅱ的检测波长为276 nm;流速：1.0 ml/min;柱温：室温;进样量：20 μl。结果 歙白术中白术内酯Ⅱ的含量显著高于其他产地白术。结论 白术内酯类成分可作为不同产地白术质量的评价指标。     

顶空进样-气相色谱-质谱法测定芪白平肺胶囊中挥发性成分

目的 测定芪白平肺胶囊中挥发性成分。方法 采用顶空进样-气相色谱-质谱联用技术,并通过所用质谱库检索研究其挥发性化学成分组成,用面积归一化法确定各成分的相对百分含量。结果 共分辨出68个色谱峰,鉴定出53个化学成分,约占总挥发性成分含量的90.75%,主要挥发性成分为酯类(38.58%)、酸类(22.97%)、杂环类(13.54%)、醛类(8.75%)、醇类(2.84%)、醚类(2.71%)、芳烃类(0.74%)和酮类(0.62%)物质,其中含量最高的是乙酸乙酯(25.54%),其次为乙酸(11.79%),含量较高的为2-甲基丁醛(7.00%),2-氨基丁酸(6.83%),乙酸丙酯(5.60%),2,3-二羟基丙酸(3.45%),糠醛(3.08%),5-甲基糠醛(3.05%),2-甲基四氢呋喃-3-酮(2.82%),2-乙酰基呋喃(2.54%),甲基环氧丙烷(2.03%),等。结论 所建立的方法分离效果较好,能够准确鉴定芪白平肺胶囊中主要挥发性成分。     

Segmental hair analysis for flunitrazepam and 7-aminoflunitrazepam in users: a comparison to existing literature

The availability of more quantitative data on flunitrazepam (FLU) and 7-aminoflunitrazepam (7AF) would aid in obtaining a better understanding of the interpretation of FLU concentrations in human hair. The purpose of this study was to provide concentrations of FLU and 7AF in hair segments of 22 FLU users. Quantitative data regarding hair concentrations of FLU and 7AF from various types of cases were also reviewed to give a comprehensive overview of the comparability of different studies. Three to six 1 cm segments of scalp hair from 22 FLU users were analyzed by a liquid chromatography–tandem mass spectrometry (LC–MS/MS) method. FLU and its metabolite were confirmed in the hair segments from all cases. Concentrations of FLU and 7AF in the segments ranged from 0.01–0.16 ng/mg (median of 0.03) and 0.01–0.34 ng/mg (median of 0.09), respectively. Most cases had FLU and 7AF distributions along the hair segments that were suggestive of repeated drug use. A summary of the published concentrations gives valuable data and can assist forensic investigators in their estimations of drug use history and patterns.

Key points

• A method using LC–MS/MS to quantify flunitrazepam and its metabolite was described.
• Segmental analysis of flunitrazepam and its metabolite in human hair was reported.
• A comprehensive overview of quantitative data was given.

     

Thermal degradation analysis of amino acids in fingerprint residue by pyrolysis GC-MS to develop new latent fingerprint developing reagents

Conventional development of latent fingerprints is compromised when the prints are decomposed by extreme temperatures, such as those encountered when a weapon cartridge is fired, an improvised explosive device is detonated, and/or in arson cases. Understanding how these extreme temperatures alter the chemical and physical properties of latent fingerprint residue could aid in the discovery of a reagent that could effectively develop these decomposed fingerprints. To mimic scenarios where fingerprints may be exposed to high heat conditions, standards of the five most abundant amino acids in fingerprint residue as well as extracted fingerprint residue were pyrolized under controlled conditions. Compounds identified as pyrolytic decomposition products were 3,6-dimethylpiperazine-2,5-dione (from alanine), maleimide, and 2,5-furandione (from aspartic acid). The pyrograms and selected ion traces show these products to hold promise as indicators of decomposed fingerprint residues and, therefore, may serve as good candidate substrates for a developing reagent.