RP-HPLC同时测定复方甘草片中4个成分的含量

目的:采用高效液相色谱法同时测定复方甘草片中吗啡、磷酸可待因、甘草苷和甘草酸的含量。方法:采用PhenomenexLuna-C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.02 mol·L-1磷酸二氢钾溶液(磷酸调pH至4.0)为流动相,梯度洗脱,流速1.0 mL·min-1,检测波长为220 nm(0～23 min,检测吗啡和可待因)、254 nm(23～50 min,检测甘草苷和甘草酸),柱温为35℃。结果:4个成分的峰面积与浓度的线性关系良好(r>0.9999);加样回收率为98.0%～100.8%。结论:该方法可用于复方甘草片中吗啡、磷酸可待因、甘草苷和甘草酸4个成分的含量测定。     

复方甘草片成瘾1例

患者 ,男 ,65岁 ,因患慢性支气管炎 ,反复咳嗽 ,口服复方甘草片 (南京第二制药厂生产 ,批号 980 5 2 5 ) 4片 ,ｔｉｄ。连续服用0 .5个月后 ,若不及时服药就会出现全身无力、烦躁焦虑、流泪、流涎、剧烈咳嗽等症状 ,若及时服用本品 ,则上述症状可在 10ｍｉｎ左右完全消失。复方甘草片是临床常用的镇咳祛痰药。其成分有 :阿片粉、甘草流浸膏等。阿片粉属麻醉药品 ,长期服用复方甘草片易成瘾。所以患者不要盲目长期服用。此外 ,可待因及含可待因的止咳药 ,长期服用亦易成瘾 ,临床医药人员均应注意复方甘草片成瘾1例@朱凤鸽$山东省德州市人民医…     

尿液LC-MS/MS检测方法快速甄别海洛因滥用者

目的獉獉:建立快速甄别海洛因滥用者的液相色谱-串级质谱法(LC-MS/MS)定性方法。方法獉獉:采用LC-MS/MS检测两个试验组即服用复方甘草片组和服用可愈糖浆后于不同时间点留取的尿样及162例海洛因滥用者的尿样,并进行描述性统计分析。结果獉獉:两个试验组尿液中均检测出吗啡、可待因、3-β-D–葡萄糖醛酸吗啡(M3G)和6-葡萄糖醛酸可待因(C6G)等吗啡类药物成分,且约在0.5-3 h浓度达到高峰,但是尿液中总吗啡和总可待因比值(Mor/Cod)是不同的。服用复方甘草片组尿液总吗啡/总可待因峰面积比值(Mor/Cod):1.61±s 0.67≤Mor/Cod<3.07±s 1.85;服用可愈糖浆组0.09±s 0.07≤Mor/Cod<0.24±s 0.12;海洛因滥用者尿液中有的可测出6-MAM,有的还可检测出海洛因或乙酰可待因原形物质,162例尿样中9例尿样Mor/Cod比值小于1且9例均检测出6-MAM外,其余均大于1。结论獉獉:本方法用于快速甄别海洛因滥用与阿片类药物使用,是相对可行的。     

罂粟组织培养中生物碱的产生

罂粟(Papaver somniferum)与有苞罂粟(P.bracteatum)是阿片生物碱可待因和吗啡的重要来源。后者的成熟蒴果含3.5%以上的蒂巴因(Thebaine)(纯度为95%),应用一般的化学方法可容易地将蒂巴因转化为可待因。罂粟的组织培养可提供该二类生物碱。本文报道,在试管内进行罂粟的细胞悬浮培养、胚状体培养与植株培养,以及其中所含生物碱的比较分析。组织培养方法:将有苞罂粟与罂粟的种子用3.0%     

阿片类药物依赖性患者尿标本中吗啡测定的色相色谱…

本文报告阿片类药物依赖性患者尿标本中同时测定吗啡和可待因的气相色谱－质谱联用法（ＧＣ－ＭＳ）的方法学研究和部分病例尿标本的测定结果。尿标本（或含吗啡和可待因的尿标准溶液）加丙烯吗啡做为内标物，经酸性条件下水解后用有机溶剂提取纯化。提取物在无水吡啶中用醋酐进行乙酰化，乙酰化衍生物进样分析。定量方法采用选择离子检测法（ＳＩＭ）。可待因、吗啡和内标物丙烯吗啡的保留时间分别为１．７４，２．３４和３．２３ｍ     

GC内标法测定复方甘草片中吗啡含量

ＧＣ内标法测定复方甘草片中吗啡含量陕西省药品检验所西安７１００６１郝武常高海复方甘草片每片中吗啡含量仅为０．４ｍｇ，其含量测定已有ＨＰＬＣ法［１］，但该法干扰大，时间长，准确性差。本文建立了气相色谱内标法，以月桂氮酮为内标物测定其吗啡含量，样品测定结...     

两种甘草酸含量测定方法对复方甘草片生产质量的影响

目的采用2010版《中国药典》中甘草浸膏和复方甘草片项下甘草酸含量测定的两种方法进行比较,探讨两种方法对复方甘草片中甘草酸含量测定结果是否有影响。方法参照2010版《中国药典》中甘草浸膏和复方甘草片项下甘草酸含量测定的方法对三种甘草浸膏和三种复方甘草片中甘草酸含量进行测定比较。结果甘草酸含量通过两种方法的测定,结果显示,甘草浸膏项下的方法测得的甘草酸含量高出复方甘草片项下的方法测得的含量1.4%左右。结论通过两种方法比较,结果差距大,为确保复方甘草片的质量,建议甘草浸膏和复方甘草片质量标准统一采用复方甘草片中甘草酸含量测定的方法。     

可待因复方制剂所致的不良反应

可待因(Codeine)是从罂粟属植物中分离出来的一种天然阿片类生物碱。进入人体的可待因约有10%经代谢转化成吗啡,其药理作用与吗啡相似,但呼吸抑制作用较吗啡轻,成瘾性也较吗啡弱,被联合国列为十种成瘾性较低的麻醉药品之一,其复方制剂被临床广泛的应用于无痰干咳、剧烈和频繁的咳嗽以及中度以上的疼痛。近年来,由可待因复方制剂引起的不良反应事件报道逐年增多,2013年2月20日,美国食     

国家发改委调整部分麻醉药品价格

2013年12月30日,国家发展和改革委员会办公厅发布《关于调整部分麻醉药品价格的通知》,决定自即日起,调整阿片粉等9种麻醉药品原料药最高出厂价格,调整复方樟脑酊等9种麻醉药品最高出厂价格和最高零售价格。《通知》说,为疏导麻醉药品初始原料价格调整的影响,保证相关药品生产供应,按照《药品政府定价办法》及有关政策规定,决定将原料药阿片粉的最高出厂价格确定为每公斤1383元,吗啡每公斤13998元,可待因每公斤10880元等.     

罂粟样品中阿片成分的分析

<正> 近年来,随着毒品问题的日益泛滥,在一些个体食品摊点中出现了用罂粟壳作火锅调料的现象。为此我们对从陕西、贵州及河南三个省收集来的罂粟果实中的几个主要部分罂粟壳、罂粟籽及附带的罂粟杆中的阿片成分进行了分析;并建立了一个比较合理的分析方法。首先用酸浸泡粉碎后的样品,取出酸液后调成碱性并用含内标的有机溶剂提取,提取溶剂挥干后用甲醇定溶,用GC/FID进行分析并用内标法计算含量。该方法简变可靠,对吗啡、可待因、蒂巴因及罂粟碱的相对偏差分别为8.2%、3.0%、1.8%和1.4%,因而适用于作普查时对大量样品     

市售复方甘草片的质量评价

目的 对市售复方甘草片的质量进行分析评价。方法 依据现行法定标准对17个生产企业的60批复方甘草片进行检验，并针对性地建立气相色谱法对样品中樟脑、反式茴香脑进行检测（标准中缺少针对挥发性组分的质量控制指标）。结果 按照法定标准检验60批复方甘草片，合格率为100%；60批样品每片含樟脑含量为0.073~1.393 mg，均未达到理论限度值（每片1.54~2.30 mg）；每片含反式茴香脑含量为0.000~1.569 mg，26批达到理论限度值（每片1.28~1.92 mg）。结论 60批复方甘草片均符合法定标准，总体质量良好；但各厂家的复方甘草片中樟脑、反式茴香脑含量存在较大差异，现行标准无法较好地反映出该品种的实际质量优劣，建议相关部门加强监管并修订完善质量标准。     

复方甘草片中樟脑的含量测定及稳定性考察

目的建立气相色谱法测定复方甘草片中樟脑含量的方法,并以恒温加速试验评价其稳定性。方法以萘为内标,GC法测定樟脑含量。25℃恒温加速试验,每10d取样1次,记录平均片重,测定樟脑的含量,并观察其色泽、气味。结果该测定方法是简便可行的。结论本实验为复方甘草片中樟脑的分析提供了一种准确可靠的检测方法,贮存时间和温度都会影响其稳定。     

不同厂家复方丹参片的有效成分含量考察

目的 考察复方丹参片有效成分含量的厂间一致性与批间稳定性.方法 采用高效液相色谱法测定A,B,C 3个厂家、不同批次复方丹参片有效成分丹参酮ⅡA和丹酚酸B的含量,分析含量变化情况.结果 3个厂家共18个批次样品有效成分含量均符合中国药典规定.除B厂和C厂产品在丹参酮ⅡA含量上存在明显差异外,各厂产品之间在丹参酮ⅡA和丹酚酸B含量上无明显不同.但有效成分含量随批次波动较大,各厂家6批次样品中有效成分丹参酮ⅡA、丹酚酸B含量变异系数分别为11.9%～22.9%和13.8%～26.5%.结论 受检厂家复方丹参片有效成分含量符合药典标准,同一厂家生产的复方丹参片有效成分含量批间稳定性差.     

复方丹参片的临床应用及质量情况调查与分析

目的：了解和分析市场中复方丹参片产品质量状况和在临床应用情况,探讨中药药物资源的合理利用。方法：调查了解复方丹参片的临床应用情况,并依照《中华人民共和国药典》（2005版）,对随机从医药市场流通中采集的45个不同企业生产的近百批次复方丹参片质量进行实验比较和分析。结果：市场调查结果显示复方丹参片的应用数量和应用人群呈逐年上升趋势;而市场中复方丹参片产品之间质量差异很大。结论：临床应用中复方丹参片产品的质量差异过大,导致药物资源的浪费和药品不合理应用,建议进一步提高和完善复方丹参片的国家药典标准。     

HPLC法测定复方甘草片中磷酸可待因含量

目的建立复方甘草片中磷酸可待因的含量测定法。方法色谱柱:Phenomenex C8;流动相:0.05mol.L-1磷酸二氢钾溶液-0.0025mol.L-1庚烷磺酸钠水溶液-乙腈(18∶18∶5);检测波长:220nm,流速:1.5mL.min-1,进样量:10μL。结果磷酸可待因在1.998~9.990μg.mL-1范围内线性良好,r=0.9999(n=6);平均回收率为100.0%(n=9,RSD为2.0%)。结论本法灵敏度高,重复性好,结果准确。     

两批掺假复方磺胺甲(口恶)唑片的质量分析

目的:对两批掺假复方磺胺甲(口恶)唑片进行全面质量分析.方法:采用TLC法,双波长分光光度法及HPLC法对两批假劣药品进行鉴别及含量测定,并对含量测定结果进行比较.结果:两批样品均掺有杂质且所掺杂质对双波长分光光度法测定含量有影响.结论:HPLC法能够分离出杂质,测定含量结果更准确.     

Rapid, simultaneous quantification of morphine, codeine, and hydromorphone by GC/MS

Morphine, codeine, and hydromorphone were extracted from blood or serum using a one step extraction. The extract was derivatized and the trifluoroacetyl opiates were quantified by GC/MS selected ion monitoring (SIM) using nalorphine as the internal standard. Calibration curves were linear and sensitivity as low as .02 mg/L for morphine and codeine, and .08 mg/L for hydromorphone, was achieved. Urine or tissue homogenates could be processed similarly after acid hydrolysis.     

Sudden death of a heroin body packer

This report documents an unusual case in which the analysis of postmortem specimens from a female heroin body packer revealed phenomenally high concentrations of morphine, 6-monoacetylmorphine (6-MAM), caffeine, and codeine. Several condoms containing white powder had split, emptied their contents into the stomach, and then leaked into the peritoneum through a rupture in the stomach wall. Blood concentrations were: morphine, 120 mg/L; (6-MAM), 184 mg/L; codeine, 1.7 mg/L; and caffeine, 400 mg/L.     

Urinary excretion of morphine and codeine following the administration of single and multiple doses of opium preparations prescribed in Taiwan as "brown mixture"

Parallel to the "poppy-seed defense" strategy commonly reported in the United States, donors of urine samples tested positive for opiates in Taiwan often claimed the consumption of Brown Mixture (BM) as the source of the observed morphine and codeine. Because BM contains opium powder (10.0-10.5% morphine), opium tincture (0.9-1.1% morphine), or camphorated opium tincture (0.045-0.055% morphine) and is a popular remedy, and heroin use is considered a serious criminal act, the claim of BM use has to be adequately addressed. In this study, BM from seven different manufacturers (5 tablets and 2 solutions) and urine samples from alleged heroin users and volunteers with various ingestion patterns and were analyzed for their morphine and codeine contents. The analytical procedure included hydrolysis, trimethylsilylation, and gas chromatography-mass spectrometry analysis. The contents of morphine and codeine in the tablets were found to be very consistent, but with significant differences in the two BM solutions. Morphine concentrations found in urine specimens collected from volunteers ingesting BM tablets (or solutions) were always < 4000 ng/mL. The following morphine-to-codeine ([M]/[C]) ratios were observed for urine specimens with morphine concentration > or = 300 ng/mL: (A) < 3.0 for volunteers ingesting BM solution and (B) > 3.0 (mostly > 5.0) for volunteers ingesting BM tablets and alleged heroin users. It appeared that (A) BM ingestion (tablet or solution) was unlikely to result in a morphine concentration > 4000 ng/mL; and (B) [M]/[C] ratio might not be an effective parameter to differentiate heroin use from BM tablet ingestion.     

Direct and efficient liquid chromatographic‐tandem mass spectrometric method for opiates in urine drug testing – importance of 6‐acetylmorphine and reduction of analytes

Opiates comprise a class of abused drugs that is of primary interest in clinical and forensic urine drug testing. Determination of heroin, codeine, or a multi‐drug ingestion is complicated since both heroin and codeine can lead to urinary excretion of free and conjugated morphine. Liquid chromatography‐tandem mass spectrometry (LC‐MS/MS) offers advantage over gas chromatography‐mass spectrometry by simplifying sample preparation but increases the number of analytes. A method based on direct injection of five‐fold diluted urine for confirmation of morphine, morphine‐3‐glucuronide, morphine‐6‐glucuronide, codeine, codeine‐6‐glucuronide and 6‐acetylmorphine was validated using LC‐MS/MS in positive electrospray mode monitoring two transitions using selected reaction monitoring. The method was applied for the analysis of 3155 unknown urine samples which were positive for opiates in immunochemical screening. A linear response was observed for all compounds in the calibration curves covering more than three orders of magnitude. Cut off was set to 2 ng/ml for 6‐acetylmorphine and 150 ng/ml for the other analytes. 6‐Acetylmorphine was found to be effective (sensitivity 82%) in detecting samples as heroin intake. Morphine‐3‐glucuronide and codeine‐6‐glucuronide was the predominant components of total morphine and codeine, 84% and 93%, respectively. The authors have validated a robust LC‐MS/MS method for rapid qualitative and quantitative analysis of opiates in urine. 6‐Acetylmorphine has been demonstrated as a sensitive and important parameter for a heroin intake. A possible interpretation strategy to conclude the source of detected analytes was proposed. The method might be further developed by reducing the number of analytes to morphine‐3‐glucuronide, codeine‐6‐glucuronide and 6‐acetylmorphine without compromising test performance. Copyright © 2013 John Wiley & Sons, Ltd.