Methods of Analysis of Opium Alkaloids

A rapid and cost‐effective method based on dispersive liquid‐liquid microextraction coupled to injection port silylation‐gas chromatography‐mass spectrometry for determination of morphine in illicit opium

“…2 Opium contains more than 25 and alone constitute by 10% of weight of raw opium. 3 The first three alkaloids, that is, morphine, codeine and thebaine belongs to the category of phenanthrene alkaloids and are internationally controlled.…”

“…A number of analytical methods for quantitative analysis of opium alkaloids are describe in literature which includes gas chromatography-mass spectrometry (GC-MS), high-performance liquid chromatography (HPLC), and capillary electrophoresis. 3,[6][7][8][9][10][11][12][13] GC-MS is a method of choice for analysis of opium alkaloids in seized and biological material due to its high selectivity, good sensitivity, high separation efficiency, and capability of unambiguous identification by comparison of unknown spectra with the spectral libraries available in the instrument. 14 However, some of the opium alkaloids need to be chemically derivatized prior to GC-MS analysis in order increase their volatility, thermal stability, detectability, and decrease consumes large amount of potentially poisonous reagent.…”

“…14 However, some of the opium alkaloids need to be chemically derivatized prior to GC-MS analysis in order increase their volatility, thermal stability, detectability, and decrease consumes large amount of potentially poisonous reagent. 3,[15][16][17] The above limitations of silylation can be overcome by using injection port silylation (IPS) technique. Compared with traditional in-vial silylation, IPS is a gaseous phase reaction which is performed inside the hot GC or GC-MS injection port between silylating reagent and polar analyte.…”

“…Out of them morphine, codeine, thebaine, papaverine, noscapine, and narceine occur naturally in the largest amount. Morphine is the principal alkaloid of opium and alone constitute by 10% of weight of raw opium 3 . The first three alkaloids, that is, morphine, codeine and thebaine belongs to the category of phenanthrene alkaloids and are internationally controlled.…”

“…For this purpose, N,O‐Bis(trimethylsilyl)acetamide (BSA), N,O‐Bis(trimethylsilyl)trifluoroacetamide (MSTFA) are the most commonly employed silylating reagents. However, major shortcomings associated to silylation are: (a) it requires totally anhydrous conditions for the reaction as the reagent are prone to hydrolysis, (b) a lengthy reaction time of 20‐30 min is needed, (c) elevated temperature in the range of 60‐100°C is mandatory for completion of reaction, and (d) consumes large amount of potentially poisonous reagent 3,15–17 …”