- What is ICP-MS?
ICP-MS is an acronym for Inductive Coupled Plasma Mass Spectroscopy. ICP-MS is an analytical instrument that combines inductive coupled plasma technology with mass spectroscopy for elemental analysis by generation of ions. An ICP-MS combines a high temperature Inductively Coupled Plasma (ICP-MS) source with a mass spectrometer (MS). The ICP source converts the atoms of the elements in the sample to ions that are separated and detected by mass spectrometer. The ICP-MS combines multi-element capabilities with detection limits equivalent or below that of GFAA and can obtain isotopic information. The instrument is capable of detecting metals and several non-metals at parts per trillion (ppt) levels.
ICP-MS is a high-tech, fairly recent addition to elemental analysis. As a result, there are no specified processes or test methods that currently exist for this technology. The technology often continues to use more conventional instrumentation, such as atomic absorption, which has been around for hundreds of years, and is not very sensitive. However, given the precision of ICP-MS testing, the FDA has been requiring ICP-MS testing more frequently.
Given the absence of existing methodologies, companies requiring ICP-MS testing must often create an ICP-MS protocol for a method and submit the protocol along with the product to a laboratory. However, at New Jersey Laboratories, we specialize in developing and validating a custom method for your product according to your specifications, and then creating and writing an ICP-MS protocol for you. We write comprehensive protocols that are accepted by the FDA, and we work closely with our clients on the protocol, explaining our process every step of the way. Our reports are solid and withstand FDA scrutiny.
- What is elemental analysis by ICP-MS and do you perform it?
Elemental analysis is an analytical technique that can determine trace to large concentrations of elements in raw materials, finished products, excipients, API, water, etc.
Yes, we perform Elemental Analysis by ICP-MS for the following elements:
Aluminum Antimony Arsenic Boron Cadmium Calcium Chromium Copper Iron Lead Magnesium Manganese Mercury Molybdenum Nickel Palldium Phosphorus Potassium Rhodium Scandium Selenium Sodium Thallium Tin Zinc
- When is elemental analysis by ICP-MS typically used?
Effective as of January 1, 2018, the United States Pharmacopeia (USP) deleted Heavy Metals <231> methodology. Elemental analysis by ICP-MS is the preferred alternative. Products that typically require ICP-MS testing include transdermal ointments, inhalers, injectibles, capsule powders, etc.
For the safety of all consumers, manufacturers are recommended to test all raw materials and supplements for their intended use.
- How are samples prepared?
Sample preparation depends on the sample. While some water-soluble samples do not require digestion, most samples must be digested in a minimal acid solution that preserves the sample’s volatile elements. Depending on the sample, New Jersey Laboratories uses one of two types of microwave digestion systems. Microwave digestion is a technique that dissolves metals in the presence of organic molecules (i.e. carbon). This process typically requires high pressures and high temperatures in acidic conditions.
- How should samples be submitted for elemental analysis by ICP-MS?
The best way to submit samples is in two separate sterile containers – one for method development and one for validation. The sample size would depend on the specifications and requirements.
- What information must be submitted along with the samples for elemental analysis by ICP-MS?
Along with the product, clients must provide specifications, also known as target limits. The target limit is the pass-fail level at a 100%.
A protocol must be written before samples can be submitted, and in order to write a protocol, a project’s elements, specifications, and any other special instructions must be submitted via email or attachments.
Since elemental analysis by ICP-MS is not a routine analytical test, but rather, a customized process, please reach out to us to discuss your project’s needs before submitting any information.
- What types of products typically require ICP-MS testing?
Excipients, API, finished products in powder, capsules, tablets, liquid forms, empty capsules, etc.
- What is validation, and why do samples need to be validated?
During method development, different samples may behave differently under digestion, and as a result, digestion matrices and parameters may change from sample to sample. The validation process allows us to take these differences into account during analysis. Method development and validation also determine which gas modes and isotopes reduce interferences, which also allow for greater accuracy and precision of results.
- What samples need to be validated?
Because the USP has not established specific methods, all samples should be validated. When validation is not performed, accuracy and precision are not guaranteed, and results are considered NON-GMP analysis.
- Why are no specific methods established in the USP?
Since extensive method validation is required by multiple laboratories, the current USP does not specify analytical methodology for finished products or raw materials by ICP-MS. Two general chapters are published as general guidelines to utilize ICP-MS and ICP-OES in order to determine the content of elements.
- What validations does New Jersey Laboratories offer that are compliant with the USP?
1. Limit Validation: The components required to satisfy limit validation include detectability, linearity, precision for instrument methods (repeatability) and specificity.
Limit validation allows New Jersey Laboratories to report whether each element of interest either passes or fails at the specification pass/fail level. All results obtained below the specification or above the specification are estimated since accuracy is not performed.
2. Quantitative Validation: The components required to satisfy quantitative validation include accuracy, precision, specificity, limit of quantitation, range, and linearity.
The last three components are demonstrated by meeting the accuracy requirement. Accuracy is performed by spiking and recovering at 50%, 100% and 150% of the target of each element. Not all elements can be analyzed together due to interferences, and several sequences may need to be performed to obtain all required results.
- What is the validation procedure?
Once we receive the sample and all required information, our quality department will write a protocol specific for the sample based on the provided specifications. The client must approve the protocol before the validation project can be scheduled. Once the validation is completed, our quality department will review the data and write a validation report.
Once the client approves the validation report, a product-specific Standard Operating Procedure (SOP) is written and takes effect for quality control (QC) analyses. Since the chemists who perform the validation also perform the QC analyses, no additional training is required, and the New Jersey Laboratories SOP can be effective upon approval.
- How long does a validation take to complete?
Depending on the elements required, the specifications, and the method development, the validation of a single sample can take 3-6 weeks.
- Is ICP-MS equivalent to Atomic Absorption?
ICP-MS is a more advanced instrument compared to Atomic Absorption in terms of detection limits, precision, sensitivity, working range, sample throughput, data quality, reducing interferences, and ease of use. Also, ICP-MS is a multi-element instrument, which allows us to test for several elements, whereas Atomic Absorption is a single element instrument.
- High Performance Thin Layer Chromatrography (HPTLC)
- What is HPTLC?
HPTLC is a modern technique that allows the proper performance of identity tests on raw materials, such as botanicals. Unlike more conventional identification tests that used filter paper dipped into a beaker, HPTLC involves sophisticated instrumentation, standardized and documented procedures, as well as validated methods. Results can be reproduced in a CGMP environment, and meets the FDA’s requirements for 100% identification of botanicals.
HPTLC testing also allows for limit tests and impurities testing in raw materials.
- Why HPTLC?
Other techniques only allow for partial identification. Microscopy is limited to plant parts. IR techniques have difficulties with the natural variability of botanical materials, and HPLC focuses on quantitative comparisons of separated markers. Each is useful, but HPTLC is a single technique with a generally applicable approach that complies with the FDA requirement of 100% botanical identification.
- When is HPTLC testing commonly used?
HPTLC testing is primarily used to identify botanicals. We provide identification of the following botanicals:
Ajuga Turkestanica (Catalpol, Indofine, Harpagoside) Alfalfa Powder Allium sativum (Garlic) (Methionine, Arginine) Annatto Seed Powder (Lutein) Ascophyllum nodosum (Lutein) Astaagalus membranaceus Avena Sativa (Escin) Bacopa (bacoside A) Barley Grass Powder Black Cohosh ID and detection of Adulterants Bladderwrack Powder (cryptoxanthin, Fucoxanthin) Blessed Thistle (Cnicus benedictus,Costunolide) Buchu Leaf (Rutin, Caffeic acid, Chlorogenic acid) Cascara Sagrada Catuaba (Yohimbe HCl, Hyoscyamine) Cayenne Pepper (Capsaicin) Cha de bugre (Rutin, Caffeic acid, Hyperoside, Chlorogenic acid) Chamomile Flower powder Cinnamomum spp. Cissus Quadrangularis (Stigmasterol, Sitosterol) Citrus Bioflavonoids (Hesperidin, Hesperidin, Naringin, Narongernin) Cola Acuminata Coleus Forskohlii (Forskolin) Cranberry Juice Powder (Naringin, Hesperidin) Damiana (Tunera diffusa) Dandelion Root Powder Eclipta prostrada (Rutin, Caffeic acid, Hyperoside, Chlorogenic acid) Eleutherococcus senticosus (Eleutheroside E, Eleutheroside B) Eurycoma longifolia (Stigmasterol, Sitosterol) Fenugreek Seed Powder Flax Seed (Eugenol, Linalool) Foti Root (Emodin, Resveratrol) Fu Ling Polysaccharide 20% (Sclerotium, Escin) Gentian Root Powder (Oleonolic acid, Oleuropein) Ginger (gingerol) Ginkgo Biloba (Rutin, Caffeic acid, Hyperoside, Chlorogenic acid) Gotu Kola HPTLC (Asiaticoside) Grape Sed (Resveratrol, EpiCatechin) Grapefruit Fruit Powder (Naringin, Hesperidin, Hesperitin) Green Tea Extract (Camellia sinesis) Epigallocatechin Gallate, EpiCatechin Ground Cloves (Eugenol) Ground Rosemary (Rutin, Hyperoside, Chlorogenic acid, Rosmaninic acid, Indofine) Guarana Seed Powder Hawthorn Berries Powder Honokoil (Magnolia) Hoodia gordinii authentication from misbranded Hops (Humulus lupulus) Horsetail (Rutin, Caffeic acid, Hypeoside, Chlorogenic Acid) Irish Moss Powder Kelp Powder Kola Nut (Cola Acuminata) (Caffeine, Theobromine) Lemon Bioflavonoids (Eriocitrin, Naringin) Licorice root (Glycyrrhizic Acid) Licorice Root Powder Milk Thistle Mushroom White Button (Ursolic acid, Sitosterol) N-Acetyl J Acid (1 Napthol-6-Acetamido 3-Sulphonic Acid) Nettle Root Olive Leaf Extract (Olea europaea) (Oleanolic acid) Oolong Tea (Epicatechin, Epigallocatechin Gallate) Panax Ginseng (ginsenoside) Panax Ginseng (ginsenoside) (Asian) Parsley Flakes (Rutin, Caffeic acid, Hyperoside, Chlorogenic Acid) Passiflora foetida (Rutin, Caffeic acid, Hyperoside, Chlorogenic acid) Passion Flower Pausinystalia johimbe (Yohimbine HCl) Phaseolus vulgaris (Quercetin Dihydrate) Pine Bark Extract (Catechin gallate, Catechin) Polygonum cuspidatum (Resveratrol, Emodin) Psyllium Husk - Plantago (Arabinose, Galactose) Pumpkin (cucurbita pepo seed) Red Clover Powder (rutin, Hyperoside, Chlorogenic Acid, Formononetin) Rhodiola Root (Rhodiola rosea) Rosehip Powder Sage (Rutin, Caffeic Acid, Hyperoside, Chlorogenic Acid) Sarspailla Powder (Escin) Saw Palmetto Schisandra Berry Powder Siberian Ginseng Powder Silybum marianum (Silybins, Silychristin) Spirulina Spirulina Platensis (Stigmasterol, Sitosterol) St John's Wort (Hypererforin, Hypersin, Hyperoside) Star Anise and Japanese Anise Stevia Extract 90% (Stevioside, Rebaudioside A) Tribulus Terrestris in finished products (Sitosterol) Tribulus terrestris Powder Tribulus terrestris Powder (aerial parts) (sitosterol) Turmeric Root Powder (Curcuma longa) (curcumin) Uva Ursi Powder Valerian Root (Valeriana officinalis) (Valeric acid, Indofine) Wheat Grass White Ash Bark (Oleanolic acid, Oleuropein) White Kidney Bean Extract (Quercetin Dihydrate) White Tea (leaf) (Epicatechin, epigallocatechin gallate) White Willow Bark (Salicin) Wild Yam Root Powder Yerba Mate Powder
- Gas Chromatography (GC)
- What is GC?
Gas chromatography refers to the group of techniques used to separate compounds in a gas-liquid and allows volatile substances in the gas phase to be analyzed. In gas chromatography, a sample’s components are dissolved in a solvent and vaporized. By distributing the sample between two phases – a stationary phase and a mobile phase – the analytes are separated.
GC allows us to pick up small molecules in a big structure, so we often use GC to test fatty samples, which typically contain small components.
- When is GC commonly used?
GC is used in many different fields, such as pharmaceuticals, cosmetics, and even environmental toxins. Since the samples have to be volatile, human breathe, blood, saliva, and other secretions containing large amounts of organic volatiles can easily be analyzed using GC.
GC is also used to analyze air samples.
- High Performance Liquid Chromatography (HPLC)
- What is HPLC?
HPLC is a chromatographic method used to separate a mixture of compounds in order to identify, quantify, or purify each component in a mixture. It is based on the fact that individual compounds behave differently in water. HPLC separates and purifies compounds according to their polarity, or their tendency to like or dislike water.
In addition to identifying components, HPLC allows us to test mixtures for limits, impurities, and potency.
- When is HPLC commonly used?
HPLC play a critical and important role in the field of pharmaceutical industries and analysis because HPLC techniques test products and detect their raw ingredients. HPLC is particularly important in these fields because they fall under FDA regulations, which obligate all pharmaceutical companies to detect the quality of their products using the HPLC before products can be sold in the global market. Additionally, HPLC can be used to determine impurities and degradation products in bulk drug materials and pharmaceutical formulations. These benefits apply to synthetic drugs and formulas, as well as herbal medicine.
- Wet Chemistry
- What is wet chemistry?
Wet chemistry analysis is performed on liquid samples using glassware and other analytical equipment, such as UV/CIS spectrometers, infrared spectrophotometers (FTIR), and polarimeters. Wet chemistry allows us to analyze samples that are too small for other instrumental methods.
For wet chemistry, we can perform tests for lead content, color, identification, water, fats, peroxide values, titrations, oxidation, acid value, sulfur dioxide, etc.
- In what fields are products typically tested using wet chemistry?
We typically test products using wet chemistry in the biochemical and pharmaceutical fields. For example, we often test supplements, raw materials, heavy metals, botanicals, excipients, etc.
- Headspace GC for Residual Solvents
- What are residual solvents?
Residual solvents in pharmaceutical products are organic volatile compounds that are used or created when drug substances, excipients, or additives are manufactured, prepared, or packaged and stored. Residual solvents are sometimes crucial in the synthesis of drug substances. Often, residual solvents are necessary to ameliorate the quality of drug substances or excipients. However, because they have no therapeutic value, if residual solvents are not completely removed by practical manufacturing methodologies, they must be evaluated and justified.
Pharmaceutical products should contain low levels of residual solvents as determined by safety data. However, residual solvents may be harmful to human health and to the environment if their presence exceeds tolerance limits as determined by safety data. As a result, residual solvents testing has become an important quality control player in pharmaceuticals.
In recent years, testing for residual solvents has grown in demand as the demand by the FDA for such testing has increased. New Jersey Laboratories owns the latest technology in this space, called Headspace GC (HSGC). HSGC is ideal because of its ability to quantify individual solvents. Although most laboratories do basic testing on residual solvents, New Jersey Laboratories also performs more difficult tests on solvents such as poloxamers.
We are highly proficient in this area, and can walk you through every step.
- When would you commonly test for residual solvents?
Testing for residual solvents is most common in the pharmaceutical field, where manufacturers are required by regulation to ensure that pharmaceuticals are free from toxicologically significant levels of volatile organic compounds.
- What methods do you follow for residual solvents?
We perform the following methods for residual solvents:
USP Chapter Test <228> Ethylene Oxide and Dioxane <467> Organic Volatile Impurities <469> Ethylene Glycol, Diethylene Glycol, and Triethylene Glycol in Ethoxylated Substances <525> Sulfur Dioxide