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Development and Method Validation for the Determination of Norfloxacin Raw Material by UPLC)
Development and Method Validation for the Determination of Norfloxacin Raw Material by UPLC)
The Ultra Performance Liquid Chromatography (UPLC) was developed and validated for determination of Norfloxacin raw material. The chromatographic conditions using Acquity UPLC BEH C18 column, 2.1 × 100 mm, 1.7 μm, column maintained at 30 °C, using 0.1% trifluoroacetic acid solution and acetonitrile mixed by gradient system as a mobile phase, flow rate 0.4 mL/min, runtime 14 minutes per injection and PDA detector at 265 nm. The chromatographic system suitability meets the suitability requirements of the United States Pharmacopoeia 41th revision (USP41). The specificity and selectivity were proved by good separation of Norfloxacin from other related compounds including Norfloxacin related compound A, Norfloxacin related compound E, Norfloxacin related compound H, Norfloxacin related compound K and degradation products. The relationship between concentration and area under curve was linear over the range of 5 to 25 μg of Norfloxacin per mL with the correlation coefficient of 0.99998. The accuracy of the results assessed by percentage recoveries of three concentration levels i.e. 5, 15 and 25 μg/mL were 100.05, 100.83 and 101.12, respectively. The system precision, performed by 3 standard solutions gave % RSD of 0.10, 0.16 and 0.15. The intermediate precision was no statistical difference of the results when the analysts, instruments and days were changed. The variations of different batches of column, column temperature, injection volume, concentration of acid in mobile phase, and flow rate did not affect the chromatographic system suitability. Limit of detection and limit of quantitation were 0.06 and 0.18 μg/mL, respectively. The UPLC method for determination of Norfloxacin raw material is simple, specific, accurate, precise, and robust. It reduces working time and reagent expense. In addition, the advantage of using not extremely high column temperature is to prolong the column life time. Therefore, the proposed method is suitable for use as a standard method for the determination of Norfloxacin raw material. Key words: Norfloxacin, UPLC
Development and Method Validation for the Determination of Norfloxacin Raw Material by UPLC)
Development and Method Validation for the Determination of Norfloxacin Raw Material by UPLC)
Sources identification of morphine in urine using an online SPE-liquid and chromatography-tandem mass spectrometry
Sources identification of morphine in urine using an online SPE-liquid and chromatography-tandem mass spectrometry
According to The Narcotics Control Act of 2519 B.E., anybody who is detected morphine in urine at the 300 ng/ml cutoff threshold, they will be reported as the drugs user. However, opium, codeine, heroin, or morphine user can meet morphine in urine. However, 6MAM can use to identify using morphine and Codeine-morphine ratio above 1 use to identify using codeine. Thus, these sunstances can derive the sources of morphine. The aim of the present work was to derive the sources of morphine in body fluids and quantification of morphine correctly using on-line solid phase extraction-liquid chromatography-tandem mass spectrometry. morphine-d3 and 6MAM-d3 are used as internal standard. Extraction by online SPE. Separation was performed on an ion-exchange column and detected by tandem mass spectrometry with electron spray ionization, positive mode. The method was validated according to the FDA guidance. Limit of 6MAM detection is 1 ng /ml. The linear range of codeine and morphine were obtained from 100-2000 ng/mL. This developed method was successfully using for quantification of morphine in human urine and its source. Can apply the method for classification of drug user in routine job of department of medical science Keywords : Morphine, Codeine, Heroine, 6MAM, urine
Sources identification of morphine in urine using an online SPE-liquid and chromatography-tandem mass spectrometry
Sources identification of morphine in urine using an online SPE-liquid and chromatography-tandem mass spectrometry
Carcinogenic chemicals contaminated in antihypertensive medicine, Angiotensin II receptor blockers
Carcinogenic chemicals contaminated in antihypertensive medicine, Angiotensin II receptor blockers
Valsartan is an angiotensin II receptor blockers(ARBs) used to treat high blood pressure and heart failure. In 2018, the U.S. FDA recalled valsartan because of contamination of the carcinogenic chemicals called N-nitrosodimethylamine (NDMA). In Thailand, Thai FDA suspended the sale and collected both ARBs raw materials and finished products. A total of 232 samples which included losartan, valsartan, olmesartan, irbesartan, azilsartan, telmisartan and candesartan were sent to Department of Medical Sciences for the analysis of nitrosamines contamination (NDMA, N-nitrosodiethylamine; NDEA and N-nitroso-N-methyl-4-aminobutyric acid; NMBA, usingliquid chromatography-tandem mass spectrometry. It was found that Losartan rawmaterials are eight samples below the limit and five samples over the limit. Valsartan rawmaterials are three samples over the limit. Losartan finished products are four samples below the limit and forty-two samples over the limit. One-hundred and seventy samples of raw materials and finished products are free fromcontamination. The limits set by ICH for NDMA and NMBA are 96 ng while that of NDEA is 26.5 ng,based on the maximum daily dose. Thai FDA suspended the sale and their production thus patients can use the medicines with confidence and reduce unnecessary carcinogens risk. Keywords: antihypertensive drug, contamination, N-nitrosodimethylamine
Carcinogenic chemicals contaminated in antihypertensive medicine, Angiotensin II receptor blockers
Carcinogenic chemicals contaminated in antihypertensive medicine, Angiotensin II receptor blockers
Development and validation method for determination of Cannabinoids in Cannabis extract and Cannabis oral drops by HPLC [Oral Presentation]
Development and validation method for determination of Cannabinoids in Cannabis extract and Cannabis oral drops by HPLC [Oral Presentation]
Cannabis oral drops is the Cannabis extract in a suitable vegetable oil. It contains Cannabinoids, including Delta-9-tetrahydrocannabinol (Delta-9-THC) and/ or Cannabidiol (CBD). It is used for the treatment of intractable epilepsy, spasticity, nausea and vomiting. In present, the analytical method for this product is unavailable in the official pharmacopoeia. Thus, Bureau of Drug and Narcotic was necessary to developed and validated the method for determination of Delta-9-THC and CBD in Cannabis extract and Cannabis oral drops by High Performance Liquid Chromatography (HPLC). The chromatographic separation was accomplished on C18, 4.6 x 150 mm reverse-phase column. The linear gradient solutions consisted of mobile phase (A) Ammonium formate pH 3.75 with 10% acetonitrile and (B) 90% acetonitrile. The flow rate was maintained at 1.0 mL/min. The analytes were monitored at 228 nm. This method was specificity. The linearity range was obtained from 2 to 100 mcg/mL. The % recovery of accuracy of Delta-9-THC and CBD were in the range of 86-99 and 94-102%, respectively. The %RSD of repeatability and intermediate precision (different instruments and days) were not more than 2.0. The standard solution and sample solution were stable for at least 2 days. This developed method is suitable to use as standard method of Thai Pharmacopoeia for determination of Delta-9-THC and CBD in Cannabis extract and Cannabis oral drops. Keywords: Cannabinoids, Cannabis extract, Cannabis oral drops, HPLC
Development and validation method for determination of Cannabinoids in Cannabis extract and Cannabis oral drops by HPLC [Oral Presentation]
Development and validation method for determination of Cannabinoids in Cannabis extract and Cannabis oral drops by HPLC [Oral Presentation]
Proficiency Testing of Nacotics in Urine Specimens 4.0, Plus Reduce
Proficiency Testing of Nacotics in Urine Specimens 4.0, Plus Reduce
Bureau of Drug and Narcotic, Department of Medical Sciences is the sole organization in Thailand offering the proficiency testing of narcotics in urine specimens. The participating members comprise approximately 750 public and private laboratories. In the 2018 fiscal year, expenses incurred in relation to issuance of reports and relevant documents and postal services amounted to 220,000 Baht. Thus, information technology (IT) was implemented through a website of https://bdn.go.th/pt/ covering 4 programs of proficiency testing (drugs, psychotropics and narcotics as property in dispute, as well as narcotics in urine specimens). It has been found that, during a one year period, total operational costs of narcotics in urine analysis was drastically decreased by more than 140,000 Baht, equivalent to 64% cost reduction. In addition, not only time but also storage space were impressively reduced by greater than 80%. Ninety five percent of paper consumption was reduced leading to environmental friendliness. The financial breaking event could be achieved within only 2-3 years. Moreover, efficiency of confidentiality mechanism, data privacy, data transferring and evaluation have been hugely improved. This website is ready to cope with participants, networks and tests expansion in the near future. The self-tracking system can be performed by the participants themselves. Although customer satisfactory evaluation was excellent, the beneficial feedbacks and suggestions would be very important for further IT system improvement.
Proficiency Testing of Nacotics in Urine Specimens 4.0, Plus Reduce
Proficiency Testing of Nacotics in Urine Specimens 4.0, Plus Reduce
Proficiency testing services for narcotics in urine of the Bureau of Drug and Narcotic, 2014-2018
Proficiency testing services for narcotics in urine of the Bureau of Drug and Narcotic, 2014-2018
Urine drug testing process is an important step in screening drug users. To ensure that the test results are precise, accurate and reliable, it is therefore necessary that the laboratories testing should participate in the proficiency testing program with the certified unit according to ISO / IEC 17043: 2010. Bureau of Drugs and Narcotics, Department of Medical Sciences has been aunit of proficiency testing provider for narcotics in urine since the fiscal year 2003 until the present. The proficiency testing for narcotics in urine consists of two schemes, namely, scheme of screening test of narcotics in urine and confirmation testing of narcotics in urine.There are a number of participating laboratories in both the public and private sectors increased by 766 respectively in the fiscal year 2018. The prevalent narcotics, methamphetamine, morphine, marijuana, ecstasy and cocaine, were used as proficiency test samples four samples a year.Because of training courses and supervision the participating laboratories of us every year, the participants reported the accurate results increasing more than 90 percent in 2018. However, there are some members reported with the inaccurate test results therefore we will plan to develop such members further. Moreover, to meet the needs of members effectively, we have used information technology. Participants are satisfied with the service. Participants’ clientreceives fairness and increase the effectiveness of prevention and suppression of drug abuse in the country
Proficiency testing services for narcotics in urine of the Bureau of Drug and Narcotic, 2014-2018
Proficiency testing services for narcotics in urine of the Bureau of Drug and Narcotic, 2014-2018
Quality of Atropine sulfate injection and Norepinephrine bitartrate injection
Quality of Atropine sulfate injection and Norepinephrine bitartrate injection
Atropine sulfate injection and Norepinephrine bitartrate injection are drugs listed in the National List of Essential Medicines 2017 in the group of cardiovascular system drugs and antidotes. By intravenous administration, both of them were used for rescuing the patients in the case of cardiac arrest in intensive care unit (ICU). Therefore, their quality of them is important. Bureau of Drug and Narcotic perform the quality survey of Atropine sulfate injection in fiscal year 2017 and of Norepinephrine bitartrate injection in fiscal year 2018. The samples were collected from hospital and manufacturer via single window system. A total of 5 Atropine sulfate injection samples, classified into 1 registration 1 from manufacturer, a total of 13 norepinephrine bitartrate injection samples, classified into 4 registration from 4 importers, were evaluated for the content of active ingredient, pH determination, particulate matter, sterility test and bacterial endotoxins by using methods and specifications of the United States Pharmacopeia (USP39 and USP40 respectively). The analytical methods were verified for the suitability prior to sample testing. The results showed that all of samples are conformed to the requirement of all topics. It can be concluded that all of the samples surveyed are good quality. Keywords: quality, Atropine sulfate injection, Norepinephrine bitartrate injection
Quality of Atropine sulfate injection and Norepinephrine bitartrate injection
Quality of Atropine sulfate injection and Norepinephrine bitartrate injection
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