Separation of standard opiates and their analysis in pharmaceutical and illicit preparations by paired-ion reverse-phase high-pressure liquid chromatography

The separation of standard opiates in a mixture and their analysis in clandestine and pharmaceutical preparations were accomplished by PIC on a micro-Bondapak C18 column. The identification of the opiates was based on two parameters: retention times and the ratios of absorbance peaks recorded at 254 and 280 nm. No prior clean-up procedure of samples was required for analysis by this method. Baseline separation of drug components in clandestine and in pharmaceutical preparations made this method suitable for their quantitation.     

Significantly increased detection rate of drugs of abuse in urine following the introduction of new German driving licence re-granting guidelines

In this paper we present the first assessment of the new German driving licence re-granting medical and psychological assessment (MPA) guidelines by comparing over 3500 urine samples tested under the old MPA cut-offs to over 5000 samples tested under the new MPA cut-offs. Since the enzyme multiplied immunoassay technique (EMIT) technology used previously was not sensitive enough to screen for drugs at such low concentrations, as suggested by the new MPA guidelines, enzyme-linked immunosorbent assay (ELISA) screening kits were used to screen for the drugs of abuse at the new MPA cut-offs. The above comparison revealed significantly increased detection rates of drug use or exposure during the rehabilitation period as follows: 1.61, 2.33, 3.33, and 7 times higher for 11-nor-delta-9-tetrahydrocannabinol-9-carboxylic acid (THC-COOH), morphine, benzoylecgonine and amphetamine respectively. The present MPA guidelines seem to be more effective to detect non-abstinence from drugs of abuse and hence to detecting drivers who do not yet fulfil the MPA requirements to regain their revoked driving licence.     

Nail analysis for the assessment of caffeine abuse in Northwest China: A population-based study

Caffeine is the most widely consumed psychoactive agent worldwide and has the potential for abuse, but studies monitoring caffeine abuse in China are scarce. This study aims to estimate the prevalence of caffeine abuse in northwest China and investigate the correlation between caffeine and other drugs in hair and nails using an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Fingernail clippings were collected from 376 participants in northwest China to detect caffeine and 13 other illicit psychoactive drugs and their metabolites. Paired hair and nail samples were collected from 39 participants to investigate the correlation between caffeine and other drugs in hair and nails. The samples were decontaminated, pulverized, and extracted by a high-throughput nail sample preparation method and analyzed by UPLC-MS/MS. The results showed a risk of caffeine abuse in northwest China, with concentrations ranging from 0.43 to 10.6 ng/mg for healthy volunteers, 0.49–246 ng/mg for caffeine abusers, and 0.25–363 ng/mg for drug addicts in community rehabilitation centers. Caffeine was detected together with other illicit psychoactive drugs and their metabolites. Furthermore, positive detection correlations were found between hair and nail samples. This study provides a current perspective on caffeine abuse in northwest China and demonstrates the practical use of UPLC-MS/MS for the simultaneous detection of caffeine and 13 illicit psychoactive drugs and their metabolites in hair and nails. The results highlight the potential of nails as a supplementary matrix when hair samples are unavailable and emphasize the need for handling caffeine carefully given its potential for abuse.     

Risk Factors Associated with the Chronicity of High Potential for Child Abuse and Neglect

The present 4-year follow-up study involves 56 mothers who were evaluated by social agencies as being abusive and neglectful or at high risk for child abuse and neglect. The aim of the study is to analyze the relationship between psychosocial risk factors (relating to the history and current situation of the mothers) that were present at the time the families were initially recruited and the fact that some of the mothers continue to show a high potential for child abuse and neglect (chronic abuse and neglect), whereas others were able to overcome the problem (transitory abuse and neglect). Results indicate that the following variables are particularly associated with situations involving chronic problems of abuse and neglect: initial level of severity of potential for abuse and neglect; dual-parent status; a large number of children at the time of intervention (3.13 times more risk of chronicity for large families); the fact that as a child the mother herself had been placed in a foster home (3.7 times more risk); that she had been sexually abused (3.5 times more risk); and that as an adolescent she had run away from home (3.02 times more risk). Our results indicate that mothers who have a combination of more than eight risk factors are four times more likely to be in the chronic group.     

Distribution of drugs of abuse within specific regions of the human brain

Since concentration of drugs of abuse found in the brain better reflect drug concentration at their site of action, brain specimens are useful in the determination of the role of drugs of abuse in the cause of death. In order to allow for the routine use of brain specimens in this field, a comprehensive database with reliable reference values is needed and should include both post-mortem data for cases where drugs have been taken in therapeutic doses as well as for cases of overdose. In this study, a semi-automated extraction procedure, in combination with gas chromatography/mass spectrometry (GC–MS) using stable isotope internal standards was applied to yield reproducible, quantitative results which could be used to investigate the distribution patterns of drugs of abuse within specific regions of the brain, by analyzing several segments of both medulla oblongata and cerebellum. A homogenous distribution of unconjugated morphine, dihydrocodeine, and benzoylecgonine within the investigated segments of medulla oblongata or cerebellum could be found. However, when these two brain regions from the same case were compared to each other, significantly higher concentrations of unconjugated morphine, dihydrocodeine, and benzoylecgonine were found in the cerebellum than in the medulla oblongata.     

固根萃取技术在系统药、毒物分析中的应用

根据反相色谱法及离子交换色谱法的原理,研制了一种固相萃取小柱,建立了筛分系统,可以同时完成对复杂体系中酸性、中性及碱性药、毒物的一次革取净化及富集,适应于系统毒物及药物筛分工作的需要。并对筛分柱的草取机理进行了初步的实验论证。     

Quantitative determination of cocaine and heroin by Fourier transform infrared spectrophotometry

Cocaine hydrochloride salt (HCl) and heroin HCl were determined quantitatively by choosing a carbonyl absorption peak as the analytical peak and measuring absorbance versus concentration in standard KBr pellets. The effect of various additives and diluents such as starch, sugars, mannitol, caffeine, and procaine was also studied. Methods were devised to correct for interference contributions based on spectral subtraction of the interfering component or subtraction of the interfering spectral contribution based on absorbance ratios with a noninterfering spectral peak. In mixtures containing both the free base and the hydrochloride salt, the most satisfactory method for determining the concentration was by area integration of the two carbonyl peaks.     

Determination of ring- and N-substituted amphetamines as heptafluorobutyryl derivatives.

An improved derivatization method for analysing 12 ring- and N-substituted amphetamine-derivatives in body fluids or seized materials by gas chromatograph combined either with mass spectrometer, electron capture or nitrogen phosphorus detector is presented. Heptafluorobutyric anhydride is used as derivatization reagent. No heating or standing period is needed in this procedure. Most of the drugs considered were distinguishable from each other according to their retention times and all of them according to their EI mass spectra. The base peak or one of the most intense peaks in the mass spectra contained benzyl radical and the m/e values were different according to the substituent.     

Dysphoria and Hopelessness Following Battering: The Role of Perceived Control, Coping, and Self-Esteem

Coping, perceived control, dysphoria, hopelessness, and self-esteem in a sample of 100 battered women were assessed. Participants reported dysphoria and low self-esteem, but not hopelessness. High perceived control over current abuse and greater use of drugs, behavioral disengagement, denial, and self-blame as coping mechanisms were associated with increased dysphoria and low self-esteem. High expectations for control over future abuse were associated with decreased dysphoria and hopelessness and increased self-esteem. After controlling for the effects of abuse severity and low self-esteem, self-blame was a unique contributor to dysphoria and high expectations for control of future abuse were unique contributors to hopelessness. Results are discussed in terms of their implications for clinical intervention with battered women.     

Trends and pattern of drug abuse deaths in Maryland teenagers

The Office of the Chief Medical Examiner of Maryland recorded a total of 149 drug abuse deaths of teenagers aged 13-19 years between 1991 and 2006. Of these deaths, 96 (64.4%) were caused by the use of narcotic drugs only, 29 (19.5%) by both narcotics and cocaine, four (2.7%) by both narcotics and methylenedioxymethamphetamine, six (4.0%) by cocaine only, and 14 (9.4%) by volatile substances (e.g., butane, Freon, nitrous oxide, and propane). The annual death rate from drug abuse for teenagers increased from 1.4 deaths per 100,000 population in 1991 to 2.7 deaths per 100,000 population in 2006 (chi-square test for time trend, p<0.01). The increase in teenager drug abuse deaths occurred in 1999 and since has remained at a higher rate. Further analysis revealed that the increase in drug abuse deaths was attributable to a large degree to narcotic drugs, particularly heroin/morphine and methadone, and was confined to teenagers residing in the suburban and rural areas.     

Hair and urine testing to assess drugs of abuse consumption in couples undergoing assisted reproductive technology (ART)

For the first time in Europe hair and urine testing have been applied to assess drugs of abuse consumption in couples undergoing assisted reproductive technology and the eventual association of toxic habits with other lifestyle, health status and sociodemographic factors was also investigated. Couples attending five assisted reproduction centers in Rome were invited to join the study. When they presented at the Centre for the visit, they were asked to answer a structured questionnaire concerning sociodemographic characteristics and lifestyle habits, and at the same time to provide hair and urine samples. Hair and urine testing for drugs of abuse, urinary profile of principal endogenous steroids involved in fertility process (testosterone, epitestosterone, androsterone, etiocholanolone and dehydroepiandrosterone) and of alcohol and tobacco smoke biomarkers were performed with validated methodologies. Of the 594 enrolled individuals (297 couples), 352 (164 couples and 24 single individuals from the couple) completed the questionnaire and gave both hair and urine samples, apart from 3 bald men, who only gave urine samples. Urine testing showed an overall 4.8% (17 individuals) positivity to drugs of abuse: 4.2% to cannabinoids, 1.4% to cocaine and 0.85% to both drugs. Results of 4cm segment hair samples testing matched those from urine samples. Thus, taking together, results of urine and hair testing confirmed repeated use of cannabis, cocaine and both drugs in 3.7, 0.85 and 0.57% examined individuals, respectively. Drug consumers were in a statistically higher percentage active smokers and alcohol drinkers, less prone to physical activity and with a trend towards higher weight than non consumers. Finally, repeated drug consumption was associated with significant lower concentration of urinary testosterone in males and of urinary dehydroepiandrosterone in females. The findings of the present study confirm the suitability of urine testing to disclose recent drugs of abuse consumption and of hair analysis to verify repeated consumption. Association between different toxic habits and sedentary lifestyle is also substantiated by the obtained results in our cohort of couples attending assisted reproduction centers.     

Preliminary Studies on the Absorbance Ratio Method Used to Determining the Age of Stamp‐pad Ink Seal

Stamp‐pad ink seals are often placed on important documents, and determining the dating of stamp‐pad ink seal is important to assess the authenticity of a document. In this study, 20 different brands and types of stamp‐pad inks were classified by ultraviolet visible spectrophotometer. Six different brands and types of papers were classified by micro‐Fourier transform infrared spectrometer and visual spectral comparator 6000. Three different brands of stamp‐pad inks and two different types of paper were used to make diachronic samples of the seals. A method was employed to date the stamp‐pad seals by comparing absorbance ratios and inks of known age. Curves were created to show the relationship between the absorbance ratio of ink and the age of the seals. The experimental results showed that the absorbance ratio method was applicable for the relative dating of stamp‐pad ink seals in some cases where the seal was placed on the document within 10 weeks.     

应用FTIR光谱技术推断死亡时间

目的 应用傅立叶变换红外(FTIR)光谱技术分析大鼠死后组织、人体离体组织随死亡时间推移的化学降解过程,为死亡时间推断的研究提供新的途径与方法.方法 大鼠断颈处死后置于4℃、20℃、30℃环境,在不同死亡时间点提取大鼠不同组织;收集有同样死亡时间的人尸体组织,离体取材,并运用FFIR光谱仪测定不同化学基团随死后和离体后...     

The detection of cotinine in hydrolyzed meconium samples.

To date, the screening of meconium for the determination of tobacco exposure in newborns has proven difficult. It was hypothesized that cotinine forms reversible Schiff base bonds with free amino functions on proteins, therefore, hydrolysis of meconium would be necessary for the detection of 'free' cotinine. One-hundred-and-two (102) meconium samples received into our laboratory were extracted using a routine non-hydrolysis screening procedure for drugs of abuse. Separate aliquots of the specimens were hydrolyzed and re-extracted according to the same procedure. The results of the two methods were compared using a highly specific cotinine micro-plate enzyme immunoassay procedure (EIA). Of the non-hydrolyzed samples, 33% were positive for cotinine, while 79% of the hydrolyzed samples were cotinine-positive. Common drugs of abuse did not interfere with the analysis. Micro-plate EIA provides a rapid, simple and reliable screening method for the determination of cotinine in meconium following hydrolysis and extraction. In general, the meconium specimens received into our laboratory are from newborns considered to be at risk for post-natal problems due to suspected drug and/or alcohol abuse during pregnancy.     

Screening analysis for medicinal drugs and drugs of abuse in whole blood using ultra-performance liquid chromatography time-of-flight mass spectrometry (UPLC-TOF-MS)-Toxicological findings in cases of alleged sexual assault

An ultra-performance liquid chromatography time-of-flight mass spectrometry (UPLC-TOF-MS) method for simultaneous screening of 46 medicinal drugs and drugs of abuse in whole blood was developed and validated. The method includes most of the commonly used and abused drugs such as amphetamines, cocaine, benzodiazepines, and opioids. Chromatographic separation of the targeted drugs was achieved using a Waters ACQUITY UPLC coupled to a Waters Micromass LCT Premier XE time-of-flight mass spectrometer. The total chromatographic run time was 13.5min injection to injection. The estimated method LOQ is in the range of 0.06-27ng/g, which is below the therapeutic levels for each of the drugs analyzed but LSD. The extraction recovery ranged from 6% to 197% with median value 95% and mean value 82%. Matrix effect ranged from 81% suppression to 29% enhancement of the signals compared to signals obtained in the absence of biological matrix. The method was tested on 55 authentic forensic toxicology samples confirming the same positive results as found using the routine analytical procedures as well as some additional compounds. Recently there has been considerable attention paid to drug-facilitated sexual assault and the toxicological findings in these cases. As part of a pilot study to investigate the prevalence of medicinal drugs, drugs of abuse, and alcohol in victims of alleged sexual assault, biological specimens were obtained from 167 victims being examined at the Sexual Assault Center in Aarhus, Denmark. The obtained blood samples were analyzed using the novel screening method supported by additional analyses for e.g. THC and alcohol. 124 victims reported they have been drinking alcohol prior to the assault (74%). Alcohol analyses revealed 59 positive findings (48%). 35 of the cases were found positive for one or more drugs excluding alcohol (21%). 20 of the victims reported they have been subject to a drug-facilitated sexual assault (12%). For the victims suspecting drug-facilitated sexual assault, the toxicological analyses revealed four positive for alcohol and nine victims were positive for one or more drugs, with six of the victims found positive for benzodiazepines or other drugs with sedative effects. It was notable that victims tested positive for medicinal drugs and drugs of abuse as well as victims of alleged drug-facilitated sexual assault in average underwent medical examination later than the whole study population.     

Simultaneous analysis of d-3-methoxy-17-methylmorphinan and l-3-methoxy-17-methylmorphinan by high pressure liquid chromatography equipped with PDA

d-3-Methoxy-17-methylmorphinan (Dextromethorphan, DXM), which is a structural analog of morphine and codeine, has been widely used as a non-narcotic antitussive agent. It is a safe drug in therapeutic dose and does not produce analgesic effects, while its enantiomer, l-3-methoxy-17-methylmorphinan called levomethorphan (LXM) is a potent narcotic analgesic. DXM has been widely abused in Korea due to its hallucinogenic effect in large doses; therefore, the health authorities have regulated its use as a psychotropic agent since 2003. As its abuse has been serious, a possibility that DXM would be smuggled into Korea has also increased. Moreover, it has been suspected that there was the possibility of the adulteration or substitution of DXM with LXM due to their chemical similarities. Therefore, it was necessary for us to establish the enantiomeric separation of DXM and LXM. In this study, a liquid chromatographic method using a chiral column capable of separating stereoisomers of DXM as well as analyzing the major metabolites of DXM, 3-methoxymorphinan, 3-hydroxymorphinan, and 17-hydroxymethylmorphinan was developed. The validation of a method was studied through repeatability of retention times. Using this method, 32 confiscated DXM samples were analyzed to identify the enantiomers of DXM. As a result, DXM was detected in all samples and there was no evidence of the adulteration or substitution of DXM with LXM. Nevertheless, the stereochemical analysis of DXM and LXM is important not only to identify starting materials for illegal drug manufacture but also to understand the trends of abused drugs.     

Characteristics of victims of sexual abuse by gender and race in a community corrections population

The purpose of this study was to examine how victims of sexual abuse in a community corrections population differ as a result of their sex and race. Of the 19,422 participants, a total of 1,298 (6.7%) reported a history of sexual abuse and were compared with nonabused participants. The sample was analyzed by race-gender groups (White men, White women, African American men, and African American women) using univariate and logistic regression analyses, which were conducted separately for each group. White women were the most likely to report a history of sexual abuse (26.5%), followed by African American women (16.0%), White men (4.0%), and African American men (1.1%). For all groups, histories of suicidal ideation and suicide attempts were associated with a history of sexual abuse. Sexual abuse was associated with substance abuse problems for women but not the men. Cannabis dependence was associated with sexual abuse for the White women while cocaine dependence was associated with sexual abuse for the African American women. Several other variables were associated with sexual abuse for women but not men, including lower education (White women only), a history of violent offenses (White women only), and living in a shelter (African American women only). African American men tended to have higher levels of education; this was the only variable uniquely associated with either male group. Receiving psychiatric medications was associated with sexual abuse for all groups except African American men and a history of sex for drugs was associated with sexual abuse for all groups except White men. Consistent with national sample, women, particularly White women, were more likely to be victims of sexual abuse. The gender-race differences for the sociodemographic factors associated with sexual abuse, particularly the risk of substance abuse for women, suggest the need for tailored interventions for sexual abuse prevention and treatment.     

I. Community Responsibility and Action

Community is the key to successful reduction of alcohol and other drug abuse. Only at the community level can effective comprehensive response be developed that will reduce both supply of and demand for destructive psychoactive drugs. Only the community can bring about the fundamental societal changes in attitudes and behavior that will reduce significantly our demand for drugs. Only the community can develop and sustain accessible programs that over time, will successfully prevent, treat and control substance abuse. The interest of society is to create a safe, secure and healthy environment that is free of drug abuse among all its members.     

Drugs in prehistory: chemical analysis of ancient human hair

Concern about drug abuse in modern populations has led to the development of specific methods for identification of cocaine, opiates and cannabis in human hair. Drug use in prehistory can provide indirect evidence of interpopulational contact and social stratification. This paper reports drug evaluation in nineteen ancient hair samples from archaeological sites in northern Chile. Each sample was tested for the presence of traces of cocaine, opiates and cannabis, in order to establish a standard methodology for studies of drug use among prehistoric groups. Although results are negative, this absence of evidence could be due to two main causes: (1) the individuals evaluated did not use any drugs, which does not mean that other members of their cultural group did, or (2) the wide range of known drugs studied did not consider some group specific drugs, derived from local or imported plants, thus meaning that a greater drug range must be tested. In any case, our study confirms that drug testing in prehistoric samples is viable. However, in order to determine what kind of substances were used in prehistoric times new patterns that incorporate all drugs which are not part of the western pharmacopeia must be created. Finally, a methodology for the study of drug use among prehistoric groups using ancient hair samples is described.