1.Simultaneous determination of 11 opiates in hair by liquid chromatography-tandem mass spectrometry.
Ying-Ying SUN ; Ping XIANG ; Min SHEN
Acta Pharmaceutica Sinica 2011;46(12):1501-1506
The paper reports the establishment of a liquid chromatography-tandem mass spectrometry (LC-MS/MS) for simultaneous analysis of 11 opiates in hair samples, and the study of presence of opiates in the hair of active heroin addicts. About 20 mg of decontaminated and pulverized hair sample was hydrolyzed with buffer solution for 30 min, in the presence of morphine-d3 and acetylmorphine-d6 used as internal standards, and then extracted with the mixture of dichlormethane and isopropanol, separated by the Allure PFP propyl column with a mobile phase consisting of acetonitrile and 20 mmol L(-1) ammonium acetate buffer, and then analyzed by LC-MS/MS. Multiple reaction monitoring (MRM) mode was used to analyze 11 opiates. Eleven opiates showed a fairly good linearity over the corresponding range (r > 0.996 0). The detection limits were less than 0.05 ng mg(-1). The recoveries were between 47.2% and 110%, and the deviations of intra- and inter-day precision were less than 14%. Heroin, acetylmorphine, morphine, codeine, acetylcodeine and hydrocodone were detected in hair samples of 21 herion addicts. The developed method shows high sensitivity and selectivity, and is suitable for the simultaneous analysis of 11 opiates in hair samples and identify legal and illegal use of opiates.
Analgesics, Opioid
;
analysis
;
Chromatography, Liquid
;
methods
;
Codeine
;
analogs & derivatives
;
analysis
;
Hair
;
chemistry
;
Heroin
;
analysis
;
Humans
;
Hydrocodone
;
analysis
;
Limit of Detection
;
Morphine
;
analysis
;
Morphine Derivatives
;
analysis
;
Sensitivity and Specificity
;
Substance Abuse Detection
;
methods
;
Tandem Mass Spectrometry
;
methods
2.Column-switching high-performance liquid chromatographic method for the determination of morphine and O6-monoacetylmorphine in urine.
Yu-rong ZHANG ; Rong WANG ; Cheng-gong ZHANG
Journal of Forensic Medicine 2002;18(2):89-91
OBJECTIVE:
To develop a column-switching high-performance liquid chromatographic method for the determination of morphine and O6-monoacetylmorphine in urine.
METHODS:
Urine samples (1.0 ml) were spiked with 1.0 ml borate buffer, after centrifugation, 1.0 ml of supernate were injected directly into an extraction column (YWG C18 33 mm x 5.0 mm, 10 microns). After a washing step with the extraction mobile phase, the retained morphine and O6-monoacetylmorphine were flushed into the analytical column (Lichrospher 100 CN 125 mm x 4.0 mm, 5 microns) with the mobile phase CH3OH-H2O (60:40). The analytical mobile phase is CH3OH-phosphate buffer (pH6.86) (22:78). The UV detector was set at lambda 286 nm.
RESULTS:
The method shows excellent linearity from 50 to 1,600 ng/ml for morphine and from 100 to 1,600 ng/ml for O6-monoacetylmorphine. The linear correlation coefficients were > 0.999. The relative standard deviations were < 4%. The limits of detection were 40 ng/ml for both morphine and O6-monoacetylmorphine.
CONCLUSION
The method described is sensitive, rapid, reproducible, and simple.
Chromatography, High Pressure Liquid/methods*
;
Heroin Dependence/urine*
;
Humans
;
Morphine/urine*
;
Morphine Derivatives/urine*
;
Sensitivity and Specificity
3.Simultaneous determination of opioid compounds in human urine by UPLC-MS/MS.
Chang-Shu ZHAN ; Bao-Hua SHEN ; Xian-Yi ZHUO
Journal of Forensic Medicine 2010;26(3):188-191
OBJECTIVE:
To propose a method for simultaneous determination of codeine(COD), 6-monoacetyl-morphine (6-MAM), morphine (MOR), morphine-3-glucuronide (M3G) and morphine-6-glucuronide (M6G) in human urine by ultra performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS).
METHODS:
After precipitation of protein by acetonitrile, the urine samples, with added the morphine-d3 (MOR-d3) and morphine-3-Glucuronide-d3 (M3G-d3) as internal standards, were pre-treated by Sirocco protein precipitation plate, and then analyzed by UPLC-MS/MS.
RESULTS:
The limit of detection was 0.2 ng/mL for both COD and MAM, the limit of quantitation was 0.5 ng/mL for both COD and MAM. The limit of detection was 0.5 ng/mL for MOR, M3G and M6G, the limit of quantitation was 1 ng/mL for them. The linear correlation coefficients were not less than 0.9997, both the inter-day and intra-day precisions were less than 10%, the recoveries were in the range of 70.0% to 98.3%, the matrix effects were about 50.5% to 99.0%.
CONCLUSION
This proposed method is simple, rapid and accurate, it could be applied in forensic toxicological analysis.
Chromatography, Liquid/methods*
;
Codeine/urine*
;
Humans
;
Limit of Detection
;
Morphine/urine*
;
Morphine Derivatives/urine*
;
Reproducibility of Results
;
Sensitivity and Specificity
;
Substance Abuse Detection/methods*
;
Tandem Mass Spectrometry/methods*
4.The research of the heroin and its metabolites analysis in clinical samples.
Lan LIN ; Lin-chuan LIAO ; You-yi YAN
Journal of Forensic Medicine 2003;19(2):126-128
Heroin can be metabolized easily in body and the mail metabolites are 6-MAM, morphine and so on. At present, there are urine, blood, hair and so on as specimens for detection, while the analytical technology conclude TLC, GC, HPLC, GC/MS, LC/MS, IA, CE etc. In this paper, these technologies used for heroin's metabolites were viewed in order to provide some reference to the study in relative field.
Chromatography, High Pressure Liquid
;
Forensic Medicine
;
Gas Chromatography-Mass Spectrometry
;
Hair/chemistry*
;
Heroin/metabolism*
;
Heroin Dependence/metabolism*
;
Humans
;
Morphine/analysis*
;
Morphine Derivatives/analysis*
;
Substance Abuse Detection/methods*
5.Study on simultaneous dosage of morphine and codeine in Opizoic tablets by HPLC
Pharmaceutical Journal 2000;293(9):16-18
After extracting completely morphine and codeine from opizoic tablets with a mixture of 3 volumes of isopropanol and 7 volumes of chloroform, an HPLC method was used to determine simultaneously morphine and codeine in the extracts. The HPLC technique was carried out on the column Lichrosorb (4x250mm, 10m) with diode array detector or UV-detector at =285 nm and a mixture of 42 volumes of 0.24% sodium heptanesulfonat solution adjusted to pH=3.2 by phosphoric acid and 18 volumes of Acetonitrile as mobile phase at flow rate 1.0ml/min. The experimental results proved that the proposed HPLC method was rapid, specific, accurate and precise.
Morphine
;
Codeine
6.Study on simultaneous qualitative and quantitative dosage of morphine and codeine by HPLC
Pharmaceutical Journal 2000;290(6):25-26
After extracting completely morphine and codeine from liquid extract of opinum with a mixture of 3 volumes of isopropanol and 7 volumes of chloroform, an HPLC method was used to determine simultaneously morphine and codeine in the extracts. The HPLC technique was carried out on the column lichrosorb (4x250mm, 10 Mm) with diode array detector or UV- detector at landa = 285 nm and a mixture of 42 volumes of 0.24% sodium heptanesulfonat solution adjusted to pH = 3.2 by phosphoric acid and 18 volumes of Acetonitrile as mobile phase at flow rate 1.0 ml/min. The experimental results proved that the proposed HPLC method was rapid, specific, accurate and precise.
Morphine
;
Codeine
7.Acute Pulmonary Edema During a Cesarian Section - A case report .
Young Ho KIM ; Choul Hae KOO ; Seong Doo CHO ; Nam Weon SONG ; Hak Lyul KIM
Korean Journal of Anesthesiology 1991;24(5):1072-1075
Pulmonary edema may be defined broadly as excessive fluid accumulation in the interstitial and air spaces of the lung. We recently a previously healthy parturient with ritodrine treatment who suddenly developed severe pulmonary edema during a Cesarian Section under Genera) Anesthesia, For this presented cases, we believe that overloading, Ritodrine, oxytocin, ergot derivatives wi11 be the causative factors. We had good result with PEEP, diuretics, and morphines.
Anesthesia
;
Diuretics
;
Lung
;
Morphine Derivatives
;
Oxytocin
;
Pulmonary Edema*
;
Ritodrine
8.Acute Pulmonary Edema During a Cesarian Section - A case report .
Young Ho KIM ; Choul Hae KOO ; Seong Doo CHO ; Nam Weon SONG ; Hak Lyul KIM
Korean Journal of Anesthesiology 1991;24(5):1072-1075
Pulmonary edema may be defined broadly as excessive fluid accumulation in the interstitial and air spaces of the lung. We recently a previously healthy parturient with ritodrine treatment who suddenly developed severe pulmonary edema during a Cesarian Section under Genera) Anesthesia, For this presented cases, we believe that overloading, Ritodrine, oxytocin, ergot derivatives wi11 be the causative factors. We had good result with PEEP, diuretics, and morphines.
Anesthesia
;
Diuretics
;
Lung
;
Morphine Derivatives
;
Oxytocin
;
Pulmonary Edema*
;
Ritodrine
9.Determination of opiates in biological human samples by liquid chromatography-tandem mass spectrometry.
Ping XIANG ; Min SHEN ; Bao-hua SHEN ; Dong MA ; Jun BU ; Yan JIANG ; Xian-yi ZHUO
Journal of Forensic Medicine 2006;22(1):52-57
OBJECTIVE:
Liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of opiates in biological samples according to the emerging problem in drugs abuse.
METHODS:
Opiates such as heroin, 6-acetylmorphine, morphine, codeine, acetylcodeine, hydrocodone and hydromorphone were isolated from human blood, urine, oral fluid and hair using a simple extraction and consequently analyzed using LC-MS/MS. The method was evaluated by real cases.
RESULTS:
The mobile phase give the optimum separation for opiates. The detection limit of morphine in urine with dilution and liquid-liquid extraction and in hair is 10ng/mL, 0.01 ng/mL and 0.01 ng/mg, respectively.
CONCLUSION
The method is simple and rapid, offering superior sensitivity and selectivity for opiates. The target compounds comprising hydrocodone and hydromorphone enlarge the applied area.
Chromatography, Liquid
;
Codeine/analysis*
;
Forensic Medicine/methods*
;
Hair/chemistry*
;
Humans
;
Hydrocodone/analysis*
;
Hydromorphone/analysis*
;
Morphine/analysis*
;
Narcotics/analysis*
;
Reproducibility of Results
;
Saliva/chemistry*
;
Substance Abuse Detection/methods*
;
Tandem Mass Spectrometry
10.Potentiation of Morphine's Antinociception by Group II and Group III Metabotropic Glutamate Receptors Agonists on a Rat Incisional Pain.
Chang Mo KIM ; Jeong Il CHOI ; Hong Beom BAE ; Seok Jai KIM ; Sung Tae CHUNG ; Ok Hwan KIM ; Myung Ha YOON
The Korean Journal of Pain 2006;19(2):131-136
BACKGROUND: The aim of this study was to clarify the role of spinal groups II and III metabotropic glutamate receptors (mGluRs) with respect to postoperative pain at the spinal level. In addition, the nature of the pharmacological interaction between groups II and III mGluRs agonists and morphine was determined. METHODS: Catheters were inserted into the intrathecal space of male SD rats. To induce postoperative pain, an incision was made in the plantar surface of the hind paw. A pharmacological characteristic for the interaction between groups II and III mGluRs agonists and morphine was evaluated using a fixed-dose analysis. RESULTS: None of intrathecal group II and III mGluRs agonists modified the withdrawal threshold of the incisional pain. The administration of intrathecal morphine resulted in an increase of a dose dependent withdrawal threshold. A fixed-dose analysis revealed that the group III mGluRs agonist, ACPT-III, increased the antinociceptive action of morphine, while the group II mGluRs agonist, APDC, had no effect the antinociception of morphine. CONCLUSIONS: These results suggest that group II and III mGluRs may not play a direct modulatory role in the processing of postoperative pain at the spinal level. However, agonizing group III mGluRs may indirectly contributable to the potentiation of morphines antinociception in the spinal cord. Thus, the combination of morphine and a group III mGluRs agonist may be useful in the management of spinal postoperative pain.
Animals
;
Catheters
;
Drug Interactions
;
Felodipine
;
Humans
;
Male
;
Morphine
;
Morphine Derivatives
;
Pain, Postoperative
;
Rats*
;
Receptors, Metabotropic Glutamate*
;
Spinal Cord